CN101893609A - Method for measuring 2-amino-1-methyl-6-phenylimidazole [4,5-b] pyridine in animal-derived foods - Google Patents
Method for measuring 2-amino-1-methyl-6-phenylimidazole [4,5-b] pyridine in animal-derived foods Download PDFInfo
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- CN101893609A CN101893609A CN 201010111646 CN201010111646A CN101893609A CN 101893609 A CN101893609 A CN 101893609A CN 201010111646 CN201010111646 CN 201010111646 CN 201010111646 A CN201010111646 A CN 201010111646A CN 101893609 A CN101893609 A CN 101893609A
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Abstract
The invention belongs to the field of analytical chemistry, and particularly relates to a method for measuring PhIP (2-amino-1-methyl-6-phenylimidazole [4,5-b] pyridine) in animal-derived foods. PhIP in the animal-derived foods is extracted with an organic solvent and purified with a solid-phase extraction column, and the content of the PhIP is detected by high performance liquid chromatography-mass spectrometry. The invention has the advantages that a sample can be processed conveniently and quickly by using the solid-phase extraction column for purifying; and the PhIP in animal-derived foods is detected by using a high performance liquid chromatography-mass spectrometry detector, compared with an ultraviolet or a fluorescence detector, the detector can eliminate matrix interference in a better way, and thus, the nature determination is more accurate, the selectivity is higher, and the sensitivity is higher.
Description
Technical field
The invention belongs to the analytical chemistry field, the assay method of PhIP in specifically a kind of animal-derived food.
Background technology
PhIP (2-amino-1-methyl-6-phenylimidazole [4,5-b] pyridine) is a kind of " dangerous " heterocyclic amine compound, and U.S. government classified it as carcinogenic substance in 2005.The research report that U.S. scientist delivers in April, 09 claims that cooking in the process of barbecue food can produce this material, and the experiment of carrying out on one's body small white mouse shows that PhIP can bring out prostate cancer.
Animal derived food except amounts of protein is arranged, outside the amino acid etc., also may add multiple flavoring additives in the manufacturing process, comprises essence and flavoring agent, edible wet goods, so food substrate is quite complicated.External useful high performance liquid chromatography and ultraviolet or fluorescence detector detect the report of heterocyclic amine in the fried food, and the domestic report that does not still have this type of detection.
Summary of the invention
The invention provides a kind of PhIP that uses in the organic solvent extraction animal-derived food, and by the Solid-Phase Extraction column purification, the high performance liquid chromatography mass spectrum detects its content.
Particular content of the present invention is:
A kind of method of measuring PhIP in the animal-derived food, it is characterized in that: with the PhIP in the organic solvent extraction animal-derived food, and by Solid-Phase Extraction column purification extract, the high performance liquid chromatography mass spectrum detects its content, wherein, described with the PhIP in the organic solvent extraction animal-derived food, and may further comprise the steps by the Solid-Phase Extraction column purification:
(1) organic solvent extraction:
Sample 2～10g adds 30～50mL organic solvent, high-speed homogenization, stand for standby use in glass beaker;
(2) the purification extract of solid-phase extraction column:
A. the activation of solid-phase extraction column:
Respectively with 1～3mL methyl alcohol, 1～3mL deionized water, the 1～3mL0.1～stand-by solid-phase extraction column of 0.5mM ammonium acetate solution activation,
B. the purification of extract:
The sample extraction solution 1～5mL that gets after homogenate is extracted is added on the solid-phase extraction column that has activated, again with 0.1～0.5mM ammonium acetate solution and the methyl alcohol mixed solution wash-out of 1～5mL 4+6, collect whole effluent, cross the 0.45um filter membrane, the high performance liquid chromatography mass spectrophotometry;
Described high performance liquid chromatography mass spectroscopy analyzing liquid sample:
A. be moving phase with methyl alcohol and 0.1% ammonium acetate system, isocratic elution is used C8, and reverse-phase chromatographic columns such as C18 separate.
B. the ion scan mode of selecting is adopted in the mass spectrum collection.
Described animal derived food is fried chicken wing, pork etc.
Described solid-phase extraction column adopts C18, C8 or PSA bonded silica gel post.
Described extraction organic solvent is acetone, methyl alcohol or acetonitrile.
Described leaching process adopts high-speed homogenization machine or oscillator.
Described measured object is: 2-amino-1-methyl-6-phenylimidazole [4,5-b] pyridine.
Beneficial effect of the present invention: utilize the Solid-Phase Extraction column purification, sample preparation is convenient and swift, with the PhIP in high performance liquid chromatography-mass detector detection animal derived food, compare with ultraviolet, fluorescence detector, can remove matrix interference better, it is qualitative more accurate to make, and selectivity is stronger, and sensitivity is higher.
Embodiment:
Embodiment one
1. the extraction of sample
The chicken wings of baking discards bone, and chicken is pulverized through food masher, accurately takes by weighing 5.0 in the 150mL beaker, accurately adds 50mL methyl alcohol, with the homogenate of high-speed homogenization machine, leaves standstill 20 minutes, makes layering, and is to be clean.
2.C18 solid-phase extraction column activation:
Respectively with 3mL methyl alcohol, 3mL deionized water, 3mL0.1mM ammonium acetate solution drip washing C18 solid-phase extraction column.Discard effluent.
3. the purification of sample:
Get and extract good sample supernatant 1ml in the good SPE post of activation, cross post with slower speed, and, collect whole effluent with 4: 6 0.1mM of 1mL ammonium acetate solution+methanol solution wash-out.Get and cross 0.45 μ m filter membrane, last machine analysis in right amount.
4. Instrument measuring:
The liquid phase chromatogram condition test condition:
Chromatographic column Agilent Eclipse reversed-phase column, 2.1 * 100mm, 3.5 μ m
Moving phase MeOH (%)+0.1% ammonium acetate buffer salt=60+40
Flow velocity 0.3mL/min
Sampling volume 40 μ L
30 ℃ of column temperatures
The mass spectrum condition:
Ion gun Ion source ESI (Positive)
Dry gas flow velocity Drying gas flow (L/min) 10
Spray needle pressure Nebulizer pressure (psig) 35
Dry gas temperature Drying gas temperature (℃) 300
Capillary voltage Capillary voltage (V) 4000
Smash voltage Fragmentor (V) 210
Select characteristic ion 225
5. qualitative and quantitative
Qualitative: as to carry out qualitative according to the retention time and the characteristic ion of compound on chromatographic column.Characteristic ion 225.
Quantitatively: according to the characteristic ion 225 of compound, external standard method is carried out quantitatively.
Claims (6)
1. method of measuring PhIP in the animal-derived food, it is characterized in that: with the PhIP in the organic solvent extraction animal-derived food, and by Solid-Phase Extraction column purification extract, the high performance liquid chromatography mass spectrum detects its content, wherein, described with the PhIP in the organic solvent extraction animal-derived food, and may further comprise the steps by the Solid-Phase Extraction column purification:
(1) organic solvent extraction:
Sample 2～10g adds 30～50mL organic solvent, high-speed homogenization, stand for standby use in glass beaker;
(2) the purification extract of solid-phase extraction column:
A. the activation of solid-phase extraction column:
Respectively with 1～3mL methyl alcohol, 1～3mL deionized water, the 1～3mL0.1～stand-by solid-phase extraction column of 0.5mM ammonium acetate solution activation,
B. the purification of extract:
The sample extraction solution 1～5mL that gets after homogenate is extracted is added on the solid-phase extraction column that has activated, again with 0.1～0.5mM ammonium acetate solution and the methyl alcohol mixed solution wash-out of 1～5mL 4+6, collect whole effluent, cross the 0.45um filter membrane, the high performance liquid chromatography mass spectrophotometry;
Described high performance liquid chromatography mass spectroscopy analyzing liquid sample:
A. be moving phase with methyl alcohol and 0.1% ammonium acetate system, isocratic elution separates with reverse-phase chromatographic column.
B. the ion scan mode of selecting is adopted in the mass spectrum collection.
2. the method for PhIP in the described mensuration animal-derived food as claimed in claim 1, it is characterized in that: described animal derived food is fried chicken wing, pork.
3. the method for PhIP in the mensuration animal-derived food as claimed in claim 1 is characterized in that: described solid-phase extraction column adopts C18, C8 or PSA bonded silica gel post.
4. the method for PhIP in the mensuration animal-derived food as claimed in claim 1 is characterized in that: described extraction organic solvent is acetone, methyl alcohol or acetonitrile.
5. the method for PhIP in the mensuration animal-derived food as claimed in claim 1 is characterized in that: described leaching process adopts high-speed homogenization machine or oscillator.
6. the method for PhIP in the mensuration animal-derived food as claimed in claim 1, it is characterized in that: described measured object is: 2-amino-1-methyl-6-phenylimidazole [4,5-b] pyridine.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010111646 CN101893609A (en) | 2010-02-22 | 2010-02-22 | Method for measuring 2-amino-1-methyl-6-phenylimidazole [4,5-b] pyridine in animal-derived foods |
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| CN 201010111646 CN101893609A (en) | 2010-02-22 | 2010-02-22 | Method for measuring 2-amino-1-methyl-6-phenylimidazole [4,5-b] pyridine in animal-derived foods |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105606743A (en) * | 2015-11-04 | 2016-05-25 | 安徽省农业科学院农产品加工研究所 | Quantitative determination method of aminopyridine carcinogenic substances in meat products |
| CN110618217A (en) * | 2019-10-29 | 2019-12-27 | 河南工业大学 | Method for detecting heterocyclic amine substances in grease |
| CN111198233A (en) * | 2018-11-20 | 2020-05-26 | 天津科技大学 | Method for detecting PhIP content in frying oil |
-
2010
- 2010-02-22 CN CN 201010111646 patent/CN101893609A/en active Pending
Non-Patent Citations (3)
| Title |
|---|
| 《Journal of Chromatography A》 19961231 M.T. Galceran*,等 Determination of heterocyclic amines by pneumatically assisted electrospray liquid chromatography-mass spectrometry 185-194 , * |
| 《分析实验室》 20090331 武晓剑，等 高效液相色谱检测反应香精中的2-氨基-N-甲基-5-苯基咪唑并吡啶(PhIP) 方法研究 第28卷, 第3期 * |
| 《南京农业大学学报》 20080430 廖国周，等 传统肉制品中杂环胺的HPLC测定 134-139 第31卷, 第4期 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105606743A (en) * | 2015-11-04 | 2016-05-25 | 安徽省农业科学院农产品加工研究所 | Quantitative determination method of aminopyridine carcinogenic substances in meat products |
| CN111198233A (en) * | 2018-11-20 | 2020-05-26 | 天津科技大学 | Method for detecting PhIP content in frying oil |
| CN110618217A (en) * | 2019-10-29 | 2019-12-27 | 河南工业大学 | Method for detecting heterocyclic amine substances in grease |
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Inventor after: Wang Peihua Inventor after: Li Qingshan Inventor after: Feng Ying Inventor after: Yu Anmin Inventor after: Liu Pingnian Inventor after: Li Guangbin Inventor after: Chen Zhiqiang Inventor before: Wang Peihua Inventor before: Li Qingshan Inventor before: Feng Ying Inventor before: Yu Anmin Inventor before: Liu Pingnian Inventor before: Li Guangbin Inventor before: Chen Zhiqiang |
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Application publication date: 20101124 |