CN112067492A - Camel milk component detection method - Google Patents
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Abstract
The invention discloses a camel milk component detection method, and relates to the technical field of dairy product detection. The method for detecting the fat content of camel milk comprises the following steps: filtering and pasteurizing camel milk; adding ammonia water, stirring, adjusting pH to 7.5-8.8, adding trypsin, and stirring for 5-6 hr; weighing camel milk in a separation container, adding ammonia water, stirring, placing in a constant-temperature water bath at 60 ℃, adding absolute ethyl alcohol, stirring, and cooling to room temperature; adding ether into a separation container, adding petroleum ether, stirring, standing for 30-40min, layering liquid in the separation container, and transferring the ether layer into a flask; adding a compound antioxidant into a flask, and weighing after drying; the fat content was calculated. According to the detection method, the protein combined with the fat is decomposed by adding the trypsin, and the antioxidant is added, so that the fat is prevented from being oxidized during heating and drying, and the content of the fat in the camel milk is detected more accurately.
Description
Technical Field
The invention relates to the technical field of dairy product detection, relates to dairy product fat content detection, and particularly relates to a camel milk component detection method.
Background
With the development and progress of society, people pay more attention to body health, so people pay more attention to the ingredients of food. Camel milk is relatively strange to many people, but in many countries it has been considered an irreplaceable nutritional product. Besides being rich in vitamin C, camel milk also contains a large amount of unsaturated fatty acid, iron and vitamin B which are required by human bodies. Before camel milk is processed, namely after camel milk is collected, camel milk components need to be measured so that additives with proper dosage can be added in subsequent processing. The detection of camel milk components comprises the determination of the fat content in camel milk. In the prior art, there is a method for detecting fat content of thick liquid, i.e. an alkaline ether extraction method, for example, a method for measuring fat content in a frozen beverage disclosed in chinese patent CN201610235650.3, which comprises adding ammonia water and ethanol to a liquid to be measured, then adding ether and petroleum ether to extract fat, finally separating ether from petroleum ether, drying and removing ether and petroleum ether, then obtaining the fat mass in the liquid to be measured, and finally calculating the fat content. However, when the method is used for detecting the fat content in the dairy product, two problems exist, namely that part of fat and protein are combined in the dairy product, and the fat is difficult to extract by using ether and petroleum ether, so that the detection result is influenced; ② when drying the ether and petroleum ether containing fat, the fat will be oxidized under heating state, which causes the final fat amount to be inaccurate and affects the detection result.
Disclosure of Invention
In order to solve the existing problems, the invention provides a camel milk component detection method, which can more accurately detect the fat content in camel milk.
In order to achieve the above object, the present invention adopts the following aspects,
a camel milk component detection method is used for detecting the fat content in camel milk and comprises the following steps:
(1) filtering and pasteurizing newly collected camel milk;
(2) taking the camel milk sterilized in the step (1), and then adding 20% ammonia water, wherein the volume ratio of the camel milk to the ammonia water is 100: 2-3, stirring for 2-3 min;
(3) dropwise adding 10% sodium hydroxide solution into the camel milk obtained in the step (2), adjusting the pH value to 7.5-8.8, adding trypsin, wherein the mass ratio of the camel milk to the trypsin is 1000:0.5-1, then placing the camel milk and the trypsin in a constant-temperature water bath for stirring, keeping the pH value to 7.5-8.8 during stirring, keeping the temperature of the water bath to 35-39 ℃, and stirring for 5-6 hours;
(4) weighing the camel milk obtained in the step (3) and placing the camel milk into a branchIn a separation vessel of the separation device, and the weight of camel milk in the separation vessel is recorded as M0And adding 20% ammonia water again, wherein the volume ratio of the camel milk to the ammonia water is 10: 1-1.2, stirring for 2-3min, then placing the separation container in a constant temperature water bath with the temperature of 60 ℃, heating and stirring for 4-6min, then adding absolute ethyl alcohol into the separation container, wherein the volume ratio of camel milk to absolute ethyl alcohol in the separation container is 1: 1-1.2, stirring for 1-2min, and cooling to room temperature;
(5) adding diethyl ether into a separation container, wherein the volume ratio of camel milk to diethyl ether is 1:2-3, stirring for 0.5-2min, then adding petroleum ether, wherein the volume ratio of camel milk to petroleum ether is 1:2-3, stirring for 0.5-2min, standing for 30-40min, separating liquid in the separation container into an upper layer and a lower layer, sequentially forming an ether layer and a water layer from top to bottom, and transferring the ether layer into a flask; the flask was weighed before use and the weight was recorded as M1；
(6) Adding diethyl ether into a separation container, stirring for 0.5-2min, adding petroleum ether, stirring for 0.5-2min, separating the liquid in the separation container into an upper layer and a lower layer, sequentially adding an ether layer and a water layer from top to bottom, transferring the ether layer into a flask, and recording the total adding weight of diethyl ether and petroleum ether as M2；
(7) The procedure of step (6) was repeated at least 2 more times, and then the flask now containing the ether layer was weighed and recorded as M3Adding a composite antioxidant with the weight of M into a flask, heating the flask to 98-100 ℃, weighing the flask every 0.5h until the difference between the weighed weight and the last weighed weight is less than 0.1mg, and recording the last weighed weight as the dried mass as M4；
(8) According to the formula
The fat content was calculated.
Preferably, in the step (7), the complex antioxidant comprises vitamin E, bamboo leaf antioxidant, tert-butylhydroquinone and butyl hydroxy anisol, wherein the ratio of the components is 1:2-4:1-2:2-3, the adding amount of the complex antioxidant is 0.03-0.05% of the total mass of the diethyl ether and the petroleum ether in the flask, and the boiling range of the petroleum ether is 30-60 ℃.
Preferably, in the step (7), the bamboo leaf antioxidant is a high-quality food grade additive produced by the biotechnology limited of Henan Liangzhi, and the content of total flavonoids is more than or equal to 40.0%, and the content of isoorientin is more than or equal to 2.0%.
Preferably, the separating apparatus comprises a base; a first upright fixed to the base; a clamping member fixed to the first column; a separation container held on the holding member; the cylinder is fixed on the base and is positioned below the separation container; and a piston rod of the air cylinder is connected with the separation container.
Furthermore, the clamping component comprises a first connecting rod, a semicircular first clamping plate, a semicircular second clamping plate and a rubber pad, one end of the first connecting rod is fixed with the first upright post, one end of the first connecting rod is fixed with the first clamping plate, two ends of the first clamping plate and two ends of the second clamping plate are respectively provided with a connecting lug, and the first clamping plate and the second clamping plate are fixed at the connecting lugs at the two ends through bolt connecting pairs; rubber pads are fixed on the opposite curved surfaces of the first clamping plate and the second clamping plate; the separation vessel is located between the first clamping plate and the second clamping plate.
Further, the separation container includes the glass pipe, the upper end of glass pipe is equipped with the stopper, the one end of liquid return bend is gone out in the glass pipe intercommunication, the other end opening of liquid return bend is downwards, the inside of glass pipe is equipped with the rubber sliding plug that can move from top to bottom, the inner wall interference fit of rubber sliding plug and glass pipe, the rubber sliding plug lower extreme upwards opens there is the blind hole, insert first sleeve pipe in the blind hole of rubber sliding plug, first sleeve pipe lies in the outer tip of blind hole and opens and have radial first pinhole, the tip of piston rod is opened has and is cooperateed first through-hole with first pinhole, the tip of piston rod inserts first sleeve pipe to insert the bolt in first pinhole and first through-hole.
Furthermore, the central axis of the piston rod is parallel to the central axis of the glass round tube; the upper end of the first sleeve is provided with an annular bulge, and the bottom of the blind hole of the rubber movable plug is provided with an annular groove for accommodating the annular bulge at the upper end of the first sleeve.
Furthermore, a second upright post is further arranged on the base, a supporting part is fixed on the second upright post, a flask is placed on the supporting part, and the other end of the liquid outlet bent pipe is inserted into the flask mouth.
Furthermore, the support component comprises a second sleeve, a second connecting rod and a horizontal support plate, the second sleeve is provided with a radial second pin hole, the second upright post is equidistantly and radially provided with a plurality of second through holes, the second sleeve is sleeved on the second upright post, and a bolt is inserted into the second pin hole and the corresponding second through hole; one end of the second connecting rod is fixed on the outer wall of the second sleeve, the other end of the second connecting rod is fixed on the edge of the supporting plate, and the flask is placed on the supporting plate.
The invention has the advantages that:
firstly, after partial ammonia water is added for treatment, casein calcium salt is destroyed, then trypsin is added, calcium ions in the camel milk are used for protecting and activating the trypsin, and the trypsin hydrolyzes protein in the camel milk, so that fat combined with the protein is released and dispersed; subsequently, ammonia water is continuously added to further destroy proteins in the camel milk, such as fat balls coated by calcium caseinate can be released, and the fat components of the camel milk can be independently dispersed in a system for subsequent extraction;
after the ether and the petroleum ether dissolve fat, a pipette is adopted to move the ether and the petroleum ether into a drying container in a traditional mode, a special separation device is adopted in the invention, when an ether layer and a water layer are separated, a movable plug in the separation container is pushed by a cylinder to move up slowly, the ether layer and the water layer also move up slowly, the upper ether layer can be gradually discharged into a flask for drying from a liquid outlet elbow, the separation is more accurate, and the operation is simpler;
during drying, the composite antioxidant which is easily dissolved in fat is added into ether and petroleum ether in a flask, the composite antioxidant adopts vitamin E, bamboo leaf antioxidant, tert-butylhydroquinone and butyl hydroxy anisole, and the vitamin E, the bamboo leaf antioxidant, the tert-butylhydroquinone and the butyl hydroxy anisole are cooperated to promote the oxidation resistance according to a specific proportion, so that the oxidation of the fat in the drying process is inhibited; in addition, the vitamin E, the bamboo leaf antioxidant, the tert-butylhydroquinone and the butyl hydroxy anisole are all easily soluble in fat, and the boiling point is higher than the drying temperature, so that the real fat content can be obtained by directly removing the mass of the compound antioxidant when the fat content is finally calculated, and the detection result is more accurate.
Drawings
FIG. 1 is a schematic view of the structure of the separation apparatus of the present invention.
Fig. 2 is a schematic structural view of the clamping member of the present invention.
FIG. 3 is a schematic diagram of the separation vessel of the present invention.
In the figure: 1-a base; 2-a first upright; 3-clamping part, 3.1-first connecting rod, 3.2-first clamping plate, 3.3-second clamping plate, 3.4-rubber pad 3.4; 4-cylinder, 4.1-piston rod; 5-separation container, 5.1-glass round tube, 5.2-plug, 5.3-liquid outlet bent tube, 5.4 rubber sliding plug, 5.5-first sleeve and 5.6-first pin hole; 6-flask; 7-a second upright; 8-support part, 8.1-second sleeve, 8.2-second connecting rod 8.3-support plate; 9.1-second vias.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to the accompanying drawings. The following examples are only for illustrating the technical solutions of the present invention more clearly, and therefore are only examples, and the protection scope of the present invention is not limited thereby.
It is to be noted that, unless otherwise specified, technical or scientific terms used herein shall have the ordinary meaning as understood by those skilled in the art to which the invention pertains.
In the description of the present application, it is to be understood that the terms "central," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," "circumferential," and the like are used in the orientations and positional relationships indicated in the drawings for convenience in describing the invention and to simplify the description, and are not intended to indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and are therefore not to be considered limiting of the invention.
Furthermore, the terms "first", "second", etc. are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
In this application, unless expressly stated or limited otherwise, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can include, for example, fixed connections, removable connections, or integral parts; can be mechanically or electrically connected; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In this application, unless expressly stated or limited otherwise, the first feature "on" or "under" the second feature may be directly contacting the first and second features or indirectly contacting the first and second features through intervening media. Also, a first feature "on," "over," and "above" a second feature may be directly or diagonally above the second feature, or may simply indicate that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature may be directly under or obliquely under the first feature, or may simply mean that the first feature is at a lesser elevation than the second feature.
The bamboo leaf antioxidant used in the following examples is a high-quality food grade additive produced by Henan Liangzhi Biotech limited, and the content of total flavonoids is more than or equal to 40.0%, and the content of isoorientin is more than or equal to 2.0%.
As shown in fig. 1, the separating apparatus used in the following embodiments includes a base 1; a first upright 2 fixed on the base 1; a clamp member 3 fixed to the first column 2; a separation vessel 5 held by the holding member 3; the cylinder 4 is fixed on the base 1 and is positioned below the separation container 5; the piston rod 4.1 of the cylinder 4 is connected with the separation container 5.
As shown in fig. 2, the clamping component 3 includes a first connecting rod 3.1, a semicircular first clamping plate 3.2, a semicircular second clamping plate 3.3 and a rubber pad 3.4, one end of the first connecting rod 3.1 is fixed to the first upright 2, one end of the first connecting rod 3.1 is fixed to the first clamping plate 3.2, two ends of the first clamping plate 3.2 and the second clamping plate 3.3 are respectively provided with a connecting lug, and the first clamping plate 3.2 and the second clamping plate 3.3 are fixed at the connecting lug at the two ends through a bolt connection pair; rubber pads 3.4 are fixed on the opposite curved surfaces of the first clamping plate 3.2 and the second clamping plate 3.3; the separation vessel 5 is located between the first clamping plate 3.2 and the second clamping plate 3.3. The rubber mat 3.4 ensures that the separation vessel is clamped by the first clamping plate 3.2 and the second clamping plate 3.3 and effectively prevents the separation vessel from slipping, thereby avoiding affecting the separation of the ether layer.
As shown in fig. 3, the separation container 5 includes a glass round tube 5.1, the upper end of the glass round tube 5.1 is provided with a plug 5.2, the glass round tube 5.1 is communicated with one end of a liquid outlet bent tube 5.3, the other end of the liquid outlet bent tube 5.3 is opened downwards, the inside of the glass round tube 5.1 is provided with a rubber sliding plug 5.4 capable of moving up and down, the rubber sliding plug 5.4 is in interference fit with the inner wall of the glass round tube 5.1, the lower end of the rubber sliding plug 5.4 is opened upwards with a blind hole, a first sleeve 5.5 is inserted into the blind hole of the rubber sliding plug 5.4, the end of the first sleeve 5.5, which is located outside the blind hole, is provided with a first pin hole 5.6, the end of the piston rod 4.1 is provided with a first through hole matched with the first pin hole 5.6, the end of the piston rod 4.1 is inserted into the first sleeve 5.5, and a plug pin is inserted into the first.
In order to ensure that the ether layer can be easily discharged from the liquid outlet bent pipe 5.3, the piston rod 4.1 and the glass round pipe 5.1 are obliquely arranged, and in order to ensure that the glass round pipe 5.1 is not damaged when the piston rod 4.1 moves, the central axis of the piston rod 4.1 is parallel to the central axis of the glass round pipe 5.1; the upper end of first sleeve pipe 5.5 is equipped with annular protrusion to the blind hole bottom of rubber activity stopper 5.4 is opened has the bellied ring channel of annular that holds first sleeve pipe 5.5 upper end, and the cooperation between annular protrusion and the ring channel has guaranteed the transmission between first sleeve pipe 5.5 and the rubber activity stopper 5.4, avoids both to separate.
Further, a second upright post 7 is further arranged on the base 1, a supporting part 8 is fixed on the second upright post 7, a flask 6 is placed on the supporting part 8, and the other end of the liquid outlet bent pipe 5.3 is inserted into the mouth of the flask 6. The supporting part 8 comprises a second sleeve 8.1, a second connecting rod 8.2 and a horizontal supporting plate 8.3, the second sleeve 8.1 is provided with a radial second pin hole, the second upright post 7 is provided with a plurality of second through holes 9.1 in the radial direction at equal distance, the second sleeve 8.1 is sleeved on the second upright post 7, and a bolt is inserted into the second pin hole and the corresponding second through hole 9.1; one end of the second connecting rod 8.2 is fixed on the outer wall of the second sleeve 8.1, the other end of the second connecting rod 8.2 is fixed on the edge of the supporting plate 8.3, and the flask 6 is placed on the supporting plate 8.3. The second sleeve 8.1 can be adjusted in position up and down on the second upright 7, thereby adjusting the height of the support plate 8.3.
When the separation device is used, the first sleeve 5.5 and the piston rod 4.1 of the separation container 5 are fixed by a bolt, the separation container 5 is fixed by the clamping part 3, then the flask is placed on the supporting part 8, the height is adjusted, the port of the liquid outlet bent pipe 5.3 is inserted into the bottleneck of the flask 6, and the port of the liquid outlet bent pipe 5.3 is kept downward; starting the air cylinder 4, the piston rod 4.1 pushes the rubber movable plug 5.4 to move upwards slowly, and similarly, the water layer and the ether layer on the rubber movable plug 5.4 move upwards slowly, and the ether layer above the water layer can gradually enter the flask 6 from the liquid outlet elbow 5.3.
Example 1
The camel milk fat content detection method comprises the following steps:
(1) filtering and pasteurizing newly collected camel milk; (2) taking the camel milk sterilized in the step (1), and then adding 20% ammonia water, wherein the volume ratio of the camel milk to the ammonia water is 100: 3, stirring for 3 min; (3) dropwise adding 10% sodium hydroxide solution into the camel milk obtained in the step (2), adjusting the pH value to 8.0, adding trypsin, wherein the mass ratio of the camel milk to the trypsin is 1000:0.5, then placing the camel milk and the trypsin in a constant-temperature water bath for stirring, keeping the pH value to 8.0 during stirring, keeping the water bath temperature to 37 ℃, and stirring for 5 hours; (4) weighing the camel milk obtained in the step (3) and placing the camel milk in a separation container of a separation device, and recording the weight of the camel milk in the separation container as M0And adding 20% ammonia water again, wherein the volume ratio of the camel milk to the ammonia water is 10: 1.2, stirring for 3min, then placing the separation container in a constant-temperature water bath with the temperature of 60 ℃, heating and stirring for 4min, then adding absolute ethyl alcohol into the separation container, wherein the volume ratio of camel milk to absolute ethyl alcohol in the separation container is 1:1, stirring for 2min, and cooling to room temperature; (5) adding diethyl ether into a separation container, wherein the volume ratio of camel milk to diethyl ether is 1:2, stirring for 0.5min, then adding petroleum ether, wherein the volume ratio of camel milk to petroleum ether is 1:2, stirring for 2min, standing for 30min, separating liquid in the separation container into an upper layer and a lower layer, sequentially forming an ether layer and a water layer from top to bottom, and transferring the ether layer into a flask; the flask was weighed before use and the weight was recorded as M1(ii) a (6) Adding diethyl ether into a separation container, stirring for 2min, adding petroleum ether, stirring for 0.5-2min, separating the liquid in the separation container into an upper layer and a lower layer, sequentially adding an ether layer and a water layer from top to bottom, transferring the ether layer into a flask, and recording the total adding weight of diethyl ether and petroleum ether as M2(ii) a (7) The procedure of step (6) was repeated 2 more times, and then the flask now containing the ether layer was weighed and recorded as M3Adding m weight of composite antioxidant into a flask, heating the flask to 100 ℃, weighing the flask every 0.5h until the fourth timeThe difference between the weighed weight and the last weighed weight was less than 0.1mg, and the fourth weighed weight was recorded as the dried mass M4；
(8) According to the formula
The fat content was calculated.
In this embodiment, the complex antioxidant comprises vitamin E, a bamboo leaf antioxidant, tert-butylhydroquinone, and butyl hydroxy anisole, wherein the ratio of each component is 1:4:2:2, the addition amount of the complex antioxidant is 0.05% of the total mass of diethyl ether and petroleum ether in the flask, and the boiling range of the petroleum ether is 30-60 ℃.
In the embodiment, when the ether layer is separated, the separation container 5 is fixed by the clamping component 3, then the piston rod 4.1 is connected, the cylinder 4 is started, the piston rod 4.1 pushes the rubber movable plug 5.4 to move upwards slowly, and the ether layer above the rubber movable plug gradually enters the flask 6 from the liquid outlet bent pipe 5.3.
Example 2
The camel milk fat content detection method comprises the following steps:
(1) filtering and pasteurizing newly collected camel milk; (2) taking the camel milk sterilized in the step (1), and then adding 20% ammonia water, wherein the volume ratio of the camel milk to the ammonia water is 100: 3, stirring for 2 min; (3) dropwise adding 10% sodium hydroxide solution into the camel milk obtained in the step (2), adjusting the pH value to 7.5, adding trypsin, wherein the mass ratio of the camel milk to the trypsin is 1000:1, then placing the camel milk and the trypsin in a constant-temperature water bath for stirring, keeping the pH value at 7.5 during stirring, keeping the water bath temperature at 38 ℃, and stirring for 6 hours; (4) weighing the camel milk obtained in the step (3) and placing the camel milk in a separation container of a separation device, and recording the weight of the camel milk in the separation container as M0And adding 20% ammonia water again, wherein the volume ratio of the camel milk to the ammonia water is 10: 1, stirring for 3min, then placing the separation container in a constant-temperature water bath with the temperature of 60 ℃, heating and stirring for 5min, then adding absolute ethyl alcohol into the separation container, wherein the volume ratio of camel milk to absolute ethyl alcohol in the separation container is 1: 1.2, stirring for 1min, and cooling toRoom temperature; (5) adding diethyl ether into a separation container, wherein the volume ratio of camel milk to diethyl ether is 1:2, stirring for 2min, then adding petroleum ether, wherein the volume ratio of camel milk to petroleum ether is 1:3, stirring for 1min, standing for 40min, separating liquid in the separation container into an upper layer and a lower layer, sequentially forming an ether layer and a water layer from top to bottom, and transferring the ether layer into a flask; the flask was weighed before use and the weight was recorded as M1(ii) a (6) Adding diethyl ether into a separation container, stirring for 2min, adding petroleum ether, stirring for 1:2, standing for 40min, separating the liquid in the separation container into an upper layer and a lower layer, sequentially adding an ether layer and a water layer from top to bottom, transferring the ether layer into a flask, and recording the total adding weight of diethyl ether and petroleum ether as M2(ii) a (7) The procedure of step (6) was repeated 2 more times, and then the flask now containing the ether layer was weighed and recorded as M3Adding a composite antioxidant with the weight of M into a flask, heating the flask to 100 ℃, weighing the flask every 0.5h until the difference between the weight of the fifth time and the weight of the last time is less than 0.1mg, and recording the weight of the fifth time as the dry mass as M4；
(8) According to the formula
The fat content was calculated.
In this embodiment, the complex antioxidant comprises vitamin E, a bamboo leaf antioxidant, tert-butylhydroquinone, and butyl hydroxy anisole, wherein the ratio of each component is 1:3:2:3, the addition amount of the complex antioxidant is 0.05% of the total mass of diethyl ether and petroleum ether in the flask, and the boiling range of the petroleum ether is 30-60 ℃.
In the embodiment, when the ether layer is separated, the separation container 5 is fixed by the clamping component 3, then the piston rod 4.1 is connected, the cylinder 4 is started, the piston rod 4.1 pushes the rubber movable plug 5.4 to move upwards slowly, and the ether layer above the rubber movable plug gradually enters the flask 6 from the liquid outlet bent pipe 5.3.
Example 3
The camel milk fat content detection method comprises the following steps:
(1) filtering and pasteurizing newly collected camel milk; (2) taking the camel milk sterilized in the step (1), and then adding 20% ammonia water, wherein the volume ratio of the camel milk to the ammonia water is 100: 3, stirring for 3 min; (3) dropwise adding 10% sodium hydroxide solution into the camel milk obtained in the step (2), adjusting the pH value to 8.5, adding trypsin, wherein the mass ratio of the camel milk to the trypsin is 1000:1, then placing the camel milk and the trypsin in a constant-temperature water bath for stirring, keeping the pH value at 8.5 during stirring, keeping the water bath temperature at 35 ℃, and stirring for 5-6 hours; (4) weighing the camel milk obtained in the step (3) and placing the camel milk in a separation container of a separation device, and recording the weight of the camel milk in the separation container as M0And adding 20% ammonia water again, wherein the volume ratio of the camel milk to the ammonia water is 10: 1.1, stirring for 2.5min, then placing the separation container in a constant-temperature water bath with the temperature of 60 ℃, heating and stirring for 4min, then adding absolute ethyl alcohol into the separation container, wherein the volume ratio of camel milk to absolute ethyl alcohol in the separation container is 1:1, stirring for 1.5min, and cooling to room temperature; (5) adding diethyl ether into a separation container, wherein the volume ratio of camel milk to diethyl ether is 1:2, stirring for 2min, then adding petroleum ether, wherein the volume ratio of camel milk to petroleum ether is 1:2, stirring for 0.5min, standing for 40min, separating liquid in the separation container into an upper layer and a lower layer, sequentially forming an ether layer and a water layer from top to bottom, and transferring the ether layer into a flask; the flask was weighed before use and the weight was recorded as M1(ii) a (6) Adding diethyl ether into a separation container, stirring for 2min, adding petroleum ether, stirring for 2min, separating the liquid in the separation container into an upper layer and a lower layer, sequentially adding an ether layer and a water layer from top to bottom, transferring the ether layer into a flask, and recording the total adding weight of diethyl ether and petroleum ether as M2(ii) a (7) The operation of step (6) was repeated 3 more times, and then the flask now containing the ether layer was weighed and recorded as M3Adding a compound antioxidant with the weight of m into a flask, heating the flask to 100 ℃, weighing the flask every 0.5h until the weight of the fourth time is different from the weight of the last time by less than 0.1mg, and recording the weight of the fourth time as dryThe mass after drying, is recorded as M4；
(8) According to the formula
The fat content was calculated.
In this embodiment, the complex antioxidant comprises vitamin E, a bamboo leaf antioxidant, tert-butylhydroquinone, and butyl hydroxy anisole, wherein the ratio of each component is 1:4:2:2, the amount of the complex antioxidant added is 0.04% of the total mass of diethyl ether and petroleum ether in the flask, and the boiling range of the petroleum ether is 30-60 ℃.
In the embodiment, when the ether layer is separated, the separation container 5 is fixed by the clamping component 3, then the piston rod 4.1 is connected, the cylinder 4 is started, the piston rod 4.1 pushes the rubber movable plug 5.4 to move upwards slowly, and the ether layer above the rubber movable plug gradually enters the flask 6 from the liquid outlet bent pipe 5.3.
Comparative example 1
The camel milk fat content detection method comprises the following steps:
(1) filtering and pasteurizing newly collected camel milk; (2) taking the camel milk sterilized in the step (1), and then adding 20% ammonia water, wherein the volume ratio of the camel milk to the ammonia water is 100: 3, stirring for 3 min; (3) weighing the camel milk obtained in the step (2) and placing the camel milk in a separation container of a separation device, and recording the weight of the camel milk in the separation container as M0And adding 20% ammonia water again, wherein the volume ratio of the camel milk to the ammonia water is 10: 1.2, stirring for 3min, then placing the separation container in a constant-temperature water bath with the temperature of 60 ℃, heating and stirring for 4min, then adding absolute ethyl alcohol into the separation container, wherein the volume ratio of camel milk to absolute ethyl alcohol in the separation container is 1:1, stirring for 2min, and cooling to room temperature; (4) adding diethyl ether into a separation container, wherein the volume ratio of camel milk to diethyl ether is 1:2, stirring for 0.5min, then adding petroleum ether, wherein the volume ratio of camel milk to petroleum ether is 1:2, stirring for 2min, standing for 30min, separating liquid in the separation container into an upper layer and a lower layer, sequentially forming an ether layer and a water layer from top to bottom, and transferring the ether layer into a flask; the flask was weighed before use and the weight was recorded as M1(ii) a (5) Re-directional separation containerAdding diethyl ether into a container, stirring for 2min, adding petroleum ether, stirring for 0.5-2min, separating the liquid in the container into upper and lower layers, sequentially adding ether layer and water layer from top to bottom, transferring the ether layer into the flask, and recording the total adding weight of diethyl ether and petroleum ether as M2(ii) a (6) The procedure of step (5) was repeated 2 more times, and then the flask now containing the ether layer was weighed and recorded as M3Adding a composite antioxidant with the weight of M into a flask, heating the flask to 100 ℃, weighing the flask every 0.5h until the difference between the fourth weighed weight and the last weighed weight is less than 0.1mg, and recording the fourth weighed weight as the dried mass as M4；
(7) According to the formula
The fat content was calculated.
In the comparative example, the composite antioxidant comprises vitamin E, a bamboo leaf antioxidant, tert-butylhydroquinone and butyl hydroxy anisol, wherein the ratio of the components is 1:4:2:2, the adding amount of the composite antioxidant is 0.05 percent of the total mass of diethyl ether and petroleum ether in a flask, and the boiling range of the petroleum ether is 30-60 ℃.
In the comparative example, when the ether layer is separated, the separation container 5 is fixed by the clamping component 3, then the piston rod 4.1 is connected, the cylinder 4 is started, the piston rod 4.1 pushes the rubber movable plug 5.4 to move upwards slowly, and the ether layer above the rubber movable plug gradually enters the flask 6 from the liquid outlet bent pipe 5.3.
Comparative example 2
The method for detecting the fat content of the camel milk comprises the following steps:
(1) filtering and pasteurizing newly collected camel milk; (2) taking the camel milk sterilized in the step (1), and then adding 20% ammonia water, wherein the volume ratio of the camel milk to the ammonia water is 100: 3, stirring for 3 min; (3) adding 10% sodium hydroxide solution dropwise into camel milk obtained in step (2), adjusting pH to 8.0, adding trypsin, camel milk and trypsinThe mass ratio of the enzyme is 1000:0.5, then the mixture is placed in a constant-temperature water bath to be stirred, the pH value is kept to be 8.0 in the stirring process, the temperature of the water bath is kept to be 37 ℃, and the stirring time is 5 hours; (4) weighing the camel milk obtained in the step (3) and placing the camel milk in a separation container of a separation device, and recording the weight of the camel milk in the separation container as M0And adding 20% ammonia water again, wherein the volume ratio of the camel milk to the ammonia water is 10: 1.2, stirring for 3min, then placing the separation container in a constant-temperature water bath with the temperature of 60 ℃, heating and stirring for 4min, then adding absolute ethyl alcohol into the separation container, wherein the volume ratio of camel milk to absolute ethyl alcohol in the separation container is 1:1, stirring for 2min, and cooling to room temperature; (5) adding diethyl ether into a separation container, wherein the volume ratio of camel milk to diethyl ether is 1:2, stirring for 0.5min, then adding petroleum ether, wherein the volume ratio of camel milk to petroleum ether is 1:2, stirring for 2min, standing for 30min, separating liquid in the separation container into an upper layer and a lower layer, sequentially forming an ether layer and a water layer from top to bottom, and transferring the ether layer into a flask; the flask was weighed before use and the weight was recorded as M1(ii) a (6) Adding diethyl ether into a separation container, stirring for 2min, adding petroleum ether, stirring for 0.5-2min, separating the liquid in the separation container into an upper layer and a lower layer, sequentially adding an ether layer and a water layer from top to bottom, transferring the ether layer into a flask, and recording the total adding weight of diethyl ether and petroleum ether as M2(ii) a (7) The procedure of step (6) was repeated 2 more times, and the flask now containing the ether layer was weighed and recorded as M3Then the flask was heated to 100 ℃ and weighed every 0.5h until the difference between the fourth weighed weight and the last weighed weight was less than 0.1mg, and the fourth weighed weight was taken as the dried mass and is taken as M4；
(8) According to the formula
The fat content was calculated.
The boiling range of petroleum ether is 30-60 ℃.
In the comparative example, when the ether layer is separated, the separation container 5 is fixed by the clamping component 3, then the piston rod 4.1 is connected, the cylinder 4 is started, the piston rod 4.1 pushes the rubber movable plug 5.4 to move upwards slowly, and the ether layer above the rubber movable plug gradually enters the flask 6 from the liquid outlet bent pipe 5.3.
Comparative example 3
The method for detecting the fat content of the camel milk comprises the following steps:
the camel milk fat content detection method comprises the following steps:
(1) filtering and pasteurizing newly collected camel milk; (2) taking the camel milk sterilized in the step (1), and then adding 20% ammonia water, wherein the volume ratio of the camel milk to the ammonia water is 100: 3, stirring for 3 min; (3) dropwise adding 10% sodium hydroxide solution into the camel milk obtained in the step (2), adjusting the pH value to 8.0, adding trypsin, wherein the mass ratio of the camel milk to the trypsin is 1000:0.5, then placing the camel milk and the trypsin in a constant-temperature water bath for stirring, keeping the pH value to 8.0 during stirring, keeping the water bath temperature to 37 ℃, and stirring for 5 hours; (4) weighing the camel milk obtained in the step (3) and placing the camel milk in a separation container of a separation device, and recording the weight of the camel milk in the separation container as M0And adding 20% ammonia water again, wherein the volume ratio of the camel milk to the ammonia water is 10: 1.2, stirring for 3min, then placing the separation container in a constant-temperature water bath with the temperature of 60 ℃, heating and stirring for 4min, then adding absolute ethyl alcohol into the separation container, wherein the volume ratio of camel milk to absolute ethyl alcohol in the separation container is 1:1, stirring for 2min, and cooling to room temperature; (5) adding diethyl ether into a separation container, wherein the volume ratio of camel milk to diethyl ether is 1:2, stirring for 0.5min, then adding petroleum ether, wherein the volume ratio of camel milk to petroleum ether is 1:2, stirring for 2min, standing for 30min, separating liquid in the separation container into an upper layer and a lower layer, sequentially forming an ether layer and a water layer from top to bottom, and transferring the ether layer into a flask; the flask was weighed before use and the weight was recorded as M1(ii) a (6) Adding diethyl ether into a separation container, stirring for 2min, adding petroleum ether, stirring for 0.5-2min, separating the liquid in the separation container into upper and lower layers, sequentially adding ether layer and water layer from top to bottom, and transferring the ether layer to the separation containerTransferred to a flask and the total weight of diethyl ether and petroleum ether added is recorded as M2(ii) a (7) The procedure of step (6) was repeated 2 more times, and then the flask now containing the ether layer was weighed and recorded as M3Adding a composite antioxidant with the weight of M into a flask, heating the flask to 100 ℃, weighing the flask every 0.5h until the difference between the fifth weighed weight and the last weighed weight is less than 0.1mg, and recording the fifth weighed weight as the dried mass as M4；
(8) According to the formula
The fat content was calculated.
In the comparative example, the composite antioxidant comprises vitamin E, a bamboo leaf antioxidant, tert-butylhydroquinone and butyl hydroxy anisol, wherein the ratio of the components is 1:4:2:2, the adding amount of the composite antioxidant is 0.05 percent of the total mass of diethyl ether and petroleum ether in a flask, and the boiling range of the petroleum ether is 30-60 ℃.
In this comparative example, when the ether layer was separated, the upper ether layer was transferred to flask 6 by using a pipette.
The data and measured fat contents of examples 1 to 3 and comparative examples 1 to 3 are shown in Table 1. Examples 1 to 3 are all results obtained by weighing using the detection method of the present invention; comparative example 1 compared to example 1, in the detection scheme, the camel milk is not subjected to enzymolysis treatment by trypsin, and obviously, the measured result is less than that of example 1; comparative example 2 compared to example 1, in the detection scheme, the results obtained by performing enzymatic hydrolysis treatment on camel milk without using an antioxidant are less than those obtained in example 1; comparative example 3 compared to example 1, the results obtained in the detection protocol were slightly less than those of example 1, using a pipette to perform the ether layer separation. Therefore, the fat detection method of camel milk provided by the invention is more accurate.
Claims (10)
1. A camel milk component detection method is used for detecting the fat content in camel milk, and is characterized by comprising the following steps:
(1) filtering and pasteurizing newly collected camel milk;
(2) taking the camel milk sterilized in the step (1), and then adding 20% ammonia water, wherein the volume ratio of the camel milk to the ammonia water is 100: 2-3, stirring for 2-3 min;
(3) dropwise adding 10% sodium hydroxide solution into the camel milk obtained in the step (2), adjusting the pH value to 7.5-8.8, adding trypsin, wherein the mass ratio of the camel milk to the trypsin is 1000:0.5-1, then placing the camel milk and the trypsin in a constant-temperature water bath for stirring, keeping the pH value to 7.5-8.8 during stirring, keeping the temperature of the water bath to 35-39 ℃, and stirring for 5-6 hours;
(4) weighing the camel milk obtained in the step (3) and placing the camel milk in a separation container of a separation device, and recording the weight of the camel milk in the separation container as M0And adding 20% ammonia water again, wherein the volume ratio of the camel milk to the ammonia water is 10: 1-1.2, stirring for 2-3min, then placing the separation container in a constant temperature water bath with the temperature of 60 ℃, heating and stirring for 4-6min, then adding absolute ethyl alcohol into the separation container, wherein the volume ratio of camel milk to absolute ethyl alcohol in the separation container is 1: 1-1.2, stirring for 1-2min, and cooling to room temperature;
(5) adding diethyl ether into a separation container, wherein the volume ratio of camel milk to diethyl ether is 1:2-3, stirring for 0.5-2min, then adding petroleum ether, wherein the volume ratio of camel milk to petroleum ether is 1:2-3, stirring for 0.5-2min, standing for 30-40min, separating liquid in the separation container into an upper layer and a lower layer, sequentially forming an ether layer and a water layer from top to bottom, and transferring the ether layer into a flask; the flask was weighed before use and the weight was recorded as M1；
(6) Adding diethyl ether into a separation container, stirring for 0.5-2min, adding petroleum ether, stirring for 0.5-2min, separating the liquid in the separation container into upper and lower layers, sequentially adding ether layer and water layer from top to bottom, transferring the ether layer to the separation container, stirring for 0.5-2min, adding petroleum ether, stirring for 0.5-2min, standing for 30-40min, separating the liquid in the separation container into upper and lower layers, sequentially adding ether layer and water layer from top to bottom, and transferring the ether layer to the separation containerIn the flask, the total weight of diethyl ether and petroleum ether charged was recorded as M2；
(7) The procedure of step (6) was repeated at least 2 more times, and then the flask now containing the ether layer was weighed and recorded as M3Adding a composite antioxidant with the weight of M into a flask, heating the flask to 98-100 ℃, weighing the flask every 0.5h until the difference between the weighed weight and the last weighed weight is less than 0.1mg, and recording the last weighed weight as the dried mass as M4；
(8) According to the formula
The fat content was calculated.
2. The camel milk component detection method according to claim 1, wherein in the step (7), the compound antioxidant comprises vitamin E, bamboo leaf antioxidant, tert-butylhydroquinone and butyl hydroxy anisole, wherein the ratio of the components is 1:2-4:1-2:2-3, the adding amount of the compound antioxidant is 0.03-0.05% of the total mass of the diethyl ether and the petroleum ether in the flask, and the boiling range of the petroleum ether is 30-60 ℃.
3. The camel milk component detection method according to claim 2, wherein in the step (7), the bamboo leaf antioxidant is a high-quality food grade additive produced by hippophae rhamnoides biotechnology limited, wherein the content of total flavonoids is more than or equal to 40.0%, and the content of isoorientin is more than or equal to 2.0%.
4. The camel milk component detection method of claim 1, wherein said separation device comprises a base; a first upright fixed to the base; a clamping member fixed to the first column; a separation container held on the holding member; the cylinder is fixed on the base and is positioned below the separation container; and a piston rod of the air cylinder is connected with the separation container.
5. The camel milk component detection method according to claim 4, wherein the clamping component comprises a first connecting rod, a semicircular first clamping plate, a semicircular second clamping plate and a rubber pad, one end of the first connecting rod is fixed with the first upright column, one end of the first connecting rod is fixed with the first clamping plate, two ends of the first clamping plate and two ends of the second clamping plate are respectively provided with a connecting lug, and the first clamping plate and the second clamping plate are fixed at the connecting lugs at the two ends through bolt connecting pairs; rubber pads are fixed on the opposite curved surfaces of the first clamping plate and the second clamping plate; the separation vessel is located between the first clamping plate and the second clamping plate.
6. The camel milk component detection method according to claim 4, wherein the separation container comprises a round glass tube, a plug is arranged at the upper end of the round glass tube, the round glass tube is communicated with one end of the liquid outlet bent tube, the other end of the liquid outlet bent tube is downward in opening, a rubber sliding plug capable of moving up and down is arranged inside the round glass tube, the rubber sliding plug is in interference fit with the inner wall of the round glass tube, a blind hole is formed in the lower end face of the rubber sliding plug in an upward mode, a first sleeve is inserted into the blind hole of the rubber sliding plug, a first radial pin hole is formed in the end portion, located outside the blind hole, of the first sleeve, a first through hole matched with the first pin hole is formed in the end portion of the piston rod, the first sleeve is inserted into the end portion of the piston rod, and a plug pin is inserted into.
7. The camel milk component detection method according to claim 6, wherein the outer wall of the glass round tube is provided with corresponding volume scales.
8. The camel milk component detection method according to claim 6, wherein the central axis of the piston rod is parallel to the central axis of the glass round tube; the upper end of the first sleeve is provided with an annular bulge, and the bottom of the blind hole of the rubber movable plug is provided with an annular groove for accommodating the annular bulge at the upper end of the first sleeve.
9. The camel milk component detection method according to claim 6, wherein a second upright is further arranged on the base, a support part is fixed on the second upright, a flask is placed on the support part, and the other end of the liquid outlet elbow is inserted into the mouth of the flask.
10. The camel milk component detection method according to claim 9, wherein the support member comprises a second sleeve, a second connecting rod and a horizontal support plate, the second sleeve is provided with a second radial pin hole, the second upright column is provided with a plurality of second through holes in a radial direction at equal intervals, the second sleeve is sleeved on the second upright column, and a bolt is inserted into the second pin hole and the corresponding second through hole; one end of the second connecting rod is fixed on the outer wall of the second sleeve, the other end of the second connecting rod is fixed on the edge of the supporting plate, and the flask is placed on the supporting plate.
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