CN106324120A - Volatile component measuring method for Tibetan medicine heracleum millefolium diels - Google Patents
Volatile component measuring method for Tibetan medicine heracleum millefolium diels Download PDFInfo
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Abstract
The invention provides a volatile component measuring method for Tibetan medicine heracleum millefolium diels. The method adopts headspace, gaseous phase, and mass spectrum to analyze the volatile components of the powder samples for heracleum millefolium diels root, stem, leaf and flower. The method includes: 1) sample crushing; 2) headspace sample introducing, solvent-free balancing, headspace air quantitative sampling and sample introducing; 3) GC-MS system separate measuring to obtain GC-MS data and 4) processing and analyzing according to GC-MS data, after retrieval by NIST11.L mass spectrum data system, ascertaining the volatile components. The method has the effects of medicinal material crushing, simple to operate, solvent free headspace condition. The method avoids distorting the measuring information caused by different solubility of volatile components. Quick headspace sample introduction and high degree of automation enhances the efficiency and accuracy of quantitative analyses. The result is reliable, and is combined with the spectrum library to retrieve; the method quickly ascertains volatile components. Ascertaining the volatile components in heracleum millefolium diels has significances for studying the material basis of medicinal efficacy, for quality control, for exploiting modern Tibet medicine.
Description
Technical field
The invention belongs to medical material detection technique, survey particularly to a kind of head space-gas phase-mass spectrum (HS-GC-MS) multiple techniques
The method determining Tibetan medicine material decomposite leaf Radix Angelicae Pubescentis volatile ingredient.
Background technology
Decomposite leaf Radix Angelicae Pubescentis Heracleum millefolium Diels is Umbelliferae (Umbelliferae) heracleum hemsleyanum michaux, has another name called
Heracleum millefolium Diels, Chiba Radix Angelicae Pubescentis, originate in China Tibet, Qinghai, Gansu, Sichuan, Yunnan, belongs to High aititude medical material.Decomposite leaf Radix Angelicae Pubescentis passes on
Tibetan medicine effect is fast, the efficacy of a drug is strong, feature pure, natural, free of contamination, and with dry all herbal medicine, bitter in the mouth, pungent, property is put down, and dissipates swollen
Swollen, abolish knot mass in the abdomen.
Tibetan medicine material decomposite leaf Radix Angelicae Pubescentis chemical constitution study report is less.At present, only have mercy on Kaohsiung et al. report (rich Kaohsiung, Pu Fa
Ancient cooking vessel, Dong Sun Han. decomposite leaf Radix Angelicae Pubescentis and the chemical composition of long decomposite leaf Radix Angelicae Pubescentis and significance for taxonomy [J] thereof. research and development of natural products
.1995,6:16-18) 11 chemical compositions of isolation identification from the ethanol extraction of decomposite leaf Radix Angelicae Pubescentis root, wherein Coumarins becomes
Divide and have 4.So far, also there are no the research about decomposite leaf Radix Angelicae Pubescentis volatile ingredient.
Volatile ingredient is produced secondary metabolite during plant intracellular metabolic, because it has pharmacology to make
With, it is widely used in clinic and health care, it is also possible to be applied to volatile ingredient study phytoecology and plant physiology
Mechanics, therefore, the research for volatile component of plant is currently a heat subject.The analysis method of volatile ingredient
There is direct injected HPLC or GC method after liquid-liquid extraction, but its extraction purification complex operation is complicated, and volatilize in unlimited system
Property composition easily loses, and causes sample message distortion.Head space concentration method has become the sample-pretreating method of modern volatile ingredient
Main study hotspot, but traditional head space aqueous solvent is different to the dissolubility of composition in sample due to it, also results in sample
Information distortion.
Summary of the invention
The present invention gathers Tibet and produces medical material decomposite leaf Radix Angelicae Pubescentis, for solving the problems referred to above, it is provided that a kind of Tibetan medicine material decomposite leaf Radix Angelicae Pubescentis is waved
The assay method of the property sent out composition, the method uses root, stem, leaf or the flower of head space-GC-MS method for combined use qualitative determination decomposite leaf Radix Angelicae Pubescentis
Middle volatile ingredient and relative amount thereof.
For achieving the above object, the present invention is achieved through the following technical solutions: a kind of Tibetan medicine material decomposite leaf Radix Angelicae Pubescentis volatility
The assay method of composition, comprises the following steps:
1) sample comminution: take decomposite leaf Radix Angelicae Pubescentis and need measurement site, be ground into medicinal powder；
2) headspace sampling: by above-mentioned medicinal powder, is directly placed into ml headspace bottle and sealing is placed in specimen disc.Sample bottle heated flat
After weighing apparatus, take sample bottle headspace gas sample introduction by quantitative loop and enter GC-MS system；
3) GC-MS system separation detection: separate and enter Mass Spectrometer Method through gas chromatogram and obtain GC-MS data；
4) analysis of volatile components.
The solvent-free head space of medicinal powder is enriched with compared with traditional head space aqueous solvent, it is to avoid owing in sample, volatility becomes
Divide the sample message distortion that the most deliquescent difference is caused.
Wherein:
Step 1) described medicinal powder is through 200-400 mesh sieve.
Step 2) sample bottle heating equilibrium condition in described headspace sampling: sample bottle heating-up temperature is 60-200 DEG C, balance
Time is 10-120min；Quantitative loop sampling condition: quantitative loop temperature 80-180 DEG C, transmission line temperature 100-180 DEG C.
Step 3) condition of described GC-MS system separation detection:
GC conditions: HP-5 capillary tube column type elasticity chromatographic column；Carrier gas: high-purity helium, purity >=99.999%；High
Pure nitrogen gas, purity >=99.999%；Post flow 1.0ml min-1；Split sampling, split ratio 10:1, injector temperature is 200-
300℃；Solvent time delay is 3.5min.Temperature programming condition: initial temperature is 50 DEG C, keeps 2min；With 2 DEG C of min-1Speed
It is warming up to 100 DEG C, keeps 3min；Again with 4 DEG C of min-1Speed be warming up to 220 DEG C, keep 3min.
Mass Spectrometry Conditions: EI ion source, electron energy 70eV；Ion source temperature 230 DEG C；Transmission line temperature is 280 DEG C；Level Four
Bar temperature is 150 DEG C；Full scan pattern；Sweep limits: m/z 50～500.
Step 4) described analysis of volatile components: GC-MS data acquisition data from gas chromatography processing system, return with peak area
One changes method measures the most each component percentage contents；And each peak in total ion current figure is obtained mass spectrum after scanning of the mass spectrum
Figure, through NIST11.L mass spectrometric data system retrieval, determines volatile ingredient.
Preferably, sample bottle heating-up temperature is 100 DEG C, and equilibration time is 40min.
Preferably, quantitative loop temperature 120 DEG C, transmission line temperature 140 DEG C.
Preferably, injector temperature is 260 DEG C.
Preferably, medicated powder powder, after 200 mesh sieves, is directly placed into ml headspace bottle and sealing is placed in specimen disc.Sample bottle heats
Temperature is 100 DEG C, and equilibration time is 40min；Quantitative loop sampling condition: quantitative loop temperature 120 DEG C, transmission line temperature 140 DEG C.Point
Flowing to sample, split ratio 10:1, injector temperature is 260 DEG C.
The invention provides a kind of method using HS-GC-MS combination to measure Tibetan medicine decomposite leaf Radix Angelicae Pubescentis volatile ingredient, the party
Having the beneficial effects that of method:
1) medical material of headspace sampling only needs to carry out pulverization process, easy and simple to handle, and molten without adding in headspace sampling condition
Other solvents such as agent water, it is to avoid in sample, volatile ingredient different solubility causes detection information distortion.
2) to change degree fast and automatically high for this detection method, improves efficiency and the accuracy of qualitative analysis, reliable results,
Bind profile library searching, can quickly confirm volatile ingredient.
3) volatile ingredient during this detection method determines decomposite leaf Radix Angelicae Pubescentis, to study its effective substance, quality control,
The exploitations of modern Tibetan medicine etc. are significant.
4) the method can be widely applied to the qualitative analysis of other traditional Chinese medicine sample volatile ingredients.
Accompanying drawing explanation
Fig. 1 is decomposite leaf Radix Angelicae Pubescentis root volatile ingredient GC-MS total ion current figure in embodiment 1；
Fig. 2 is decomposite leaf Radix Angelicae Pubescentis stem volatile ingredient GC-MS total ion current figure in embodiment 2；
Fig. 3 is decomposite leaf Radix Angelicae Pubescentis leaf volatile ingredient GC-MS total ion current figure in embodiment 3；
Fig. 4 is decomposite leaf Radix Angelicae Pubescentis flower volatile ingredient GC-MS total ion current figure in embodiment 4.
Detailed description of the invention
For preferably explaining the present invention, below in conjunction with the accompanying drawings embodiments of the invention are described in detail.
Decomposite leaf Radix Angelicae Pubescentis used by the present invention: decomposite leaf Radix Angelicae Pubescentis medical material gathers on the spot in Gang Dui town, Gongga County, Shannan District of Tibet Autonomous Region, by
National level teaching team of pharmaceutical college of Jiangxi University of Traditional Chinese Medicine leader professor Gong Qianfeng is accredited as decomposite leaf Radix Angelicae Pubescentis.
Agents useful for same of the present invention: high-purity helium, purity >=99.999%；High pure nitrogen, purity >=99.999%.
Instrument of the present invention: Agilent 7697A automatic headspace sample injector (Agilent company, the U.S.)；7890A type gas
Chromatography (Agilent company, the U.S.)；The mono-quadrupole mass spectrometer of 5975C (Agilent company, the U.S.)；Balance: ten thousand/
Balance (Sartorius BT 224S).
Embodiment 1
The assay method of volatile ingredient in Tibetan medicine material decomposite leaf Radix Angelicae Pubescentis root, comprises the following steps:
1) sample comminution: take the root of decomposite leaf Radix Angelicae Pubescentis, is ground into medicinal powder (crossing 200 mesh sieves)；
2) headspace sampling: weigh above-mentioned medicinal powder 0.2000g, is directly placed into 20ml ml headspace bottle and sealing is placed in sample
Dish.Sample bottle heating-up temperature is 100 DEG C, and equilibration time is 40min；Take sample bottle headspace gas 1mL sample introduction and enter GC-MS system
System, quantitative loop temperature 120 DEG C, transmission line temperature 140 DEG C；
3) GC-MS system separation detection: separate through gas chromatogram and enter Mass Spectrometer Method.
Wherein, GC conditions: HP-5 capillary tube column type elasticity chromatographic column (0.25 μ m 250 μ m 30m)；Carrier gas:
High-purity helium, high pure nitrogen；Post flow 1.0ml min-1；Use split sampling, split ratio 10: 1；Injector temperature is 260
℃；Solvent time delay is 3.5min.Temperature programming condition: initial temperature is 50 DEG C (keeping 2min), with 2 DEG C of min-1Speed liter
Warm to 100 DEG C (keeping 3min), then with 4 DEG C of min-1Speed be warming up to 220 DEG C (keep 3min)；
Mass Spectrometry Conditions: EI ion source, electron energy 70eV；Ion source temperature 230 DEG C；Transmission line temperature is 280 DEG C；Level Four
Bar temperature is 150 DEG C；Full scan pattern；Sweep limits: m/z 50～500；
4) analysis of volatile components: GC-MS data acquisition data from gas chromatography processing system, surveys with areas of peak normalization method
The most each fixed component percentage contents；And each peak in total ion current figure is obtained mass spectrum after scanning of the mass spectrum, pass through
NIST11.L mass spectrometric data system retrieval, determines volatile ingredient.
The total ion current figure of decomposite leaf Radix Angelicae Pubescentis root volatile ingredient is shown in Fig. 1 respectively.Result shows, decomposite leaf Radix Angelicae Pubescentis root volatility becomes
Point be divided into out 34 kinds of materials, 7 kinds of content of material more than 5%, wherein octanal 17.177%, hexanal 15.979%, enanthaldehyde
11.118%, o-isopropyl methylbenzene 8.478%, 2-amyl furan 7.332%, 1-methyl-4-(1-Methylethyl)-Isosorbide-5-Nitrae-hexamethylene
Diene (γ-terpinene) 5.559%, terpinolene 5.391%, account for more than the 70% of volatile ingredient.
Embodiment 2
The assay method of volatile ingredient in Tibetan medicine material decomposite leaf Radix Angelicae Pubescentis stem, comprises the following steps:
1) sample comminution: take the stem of decomposite leaf Radix Angelicae Pubescentis, is ground into medicinal powder (crossing 300 mesh sieves)；
2) headspace sampling: weigh above-mentioned medicinal powder 0.2500g, is directly placed into 20ml ml headspace bottle and sealing is placed in sample
Dish.Sample bottle heating-up temperature is 60 DEG C, and equilibration time is 120min；Take sample bottle headspace gas 1mL sample introduction and enter GC-MS system
System, quantitative loop temperature 80 DEG C, transmission line temperature 100 DEG C；
3) GC-MS system separation detection: separate through gas chromatogram and enter Mass Spectrometer Method.
Wherein, GC conditions: HP-5 capillary tube column type elasticity chromatographic column (0.25 μ m 250 μ m 30m)；Carrier gas:
High-purity helium, high pure nitrogen；Post flow 1.0ml min-1；Use split sampling, split ratio 10: 1；Injector temperature is 200
℃；Solvent time delay is 3.5min.Temperature programming condition: initial temperature is 50 DEG C (keeping 2min), with 2 DEG C of min-1Speed liter
Warm to 100 DEG C (keeping 3min), then with 4 DEG C of min-1Speed be warming up to 220 DEG C (keep 3min)；
Mass Spectrometry Conditions and analysis of volatile components step are with embodiment 1.
The total ion current figure of decomposite leaf Radix Angelicae Pubescentis stem volatile ingredient is shown in Fig. 2 respectively.Decomposite leaf Radix Angelicae Pubescentis stem volatile ingredient is divided into out
41 kinds of materials, 7 kinds of content of material more than 4%, wherein trimethylbenzene methanol 10.808%, 4-isopropyl toluene 10.369%, 4-
Isopropenyl toluene 9.675%, γ-terpinene 8.339%, β-cyclocitral 5.608%, octanal 5.003%, hexanal
4.463%, account for more than the 54% of volatile ingredient.
Embodiment 3
The assay method of volatile ingredient in Tibetan medicine material decomposite leaf Radix Angelicae Pubescentis leaf, comprises the following steps:
1) sample comminution: take the leaf of decomposite leaf Radix Angelicae Pubescentis, is ground into medicinal powder (crossing 400 mesh sieves)；
2) headspace sampling: weigh above-mentioned medicinal powder 0.1500g, is directly placed into 20ml ml headspace bottle and sealing is placed in sample
Dish.Sample bottle heating-up temperature is 200 DEG C, and equilibration time is 10min；Take sample bottle headspace gas 1mL sample introduction and enter GC-MS system
System, quantitative loop temperature 180 DEG C, transmission line temperature 180 DEG C；
3) GC-MS system separation detection: separate through gas chromatogram and enter Mass Spectrometer Method.
Wherein, GC conditions: HP-5 capillary tube column type elasticity chromatographic column (0.25 μ m 250 μ m 30m)；Carrier gas:
High-purity helium, high pure nitrogen；Post flow 1.0ml min-1；Use split sampling, split ratio 10: 1；Injector temperature is 300
℃；Solvent time delay is 3.5min.Temperature programming condition: initial temperature is 50 DEG C (keeping 2min), with 2 DEG C of min-1Speed liter
Warm to 100 DEG C (keeping 3min), then with 4 DEG C of min-1Speed be warming up to 220 DEG C (keep 3min)；
Mass Spectrometry Conditions and analysis of volatile components step are with embodiment 1.
The total ion current figure of decomposite leaf Radix Angelicae Pubescentis leaf volatile ingredient is shown in Fig. 3 respectively.Decomposite leaf Radix Angelicae Pubescentis leaf volatile ingredient is divided into out
34 kinds of materials, 7 kinds of content of material near or above 4%, wherein terpinolene 15.339%, o-isopropyl benzene 11.454%, γ-
Terpinene 9.609%, (R)-(+)-limonene 9.564%, trimethylbenzene methanol 7.481%, (E)-(3,3-dimethyleyelohexane are sub-
Base)-acetaldehyde 4.936%, 2,3-dehydrogenation-1, 8-Cineole 3.986%, account for more than the 62% of volatile ingredient.
Embodiment 4
Tibetan medicine material decomposite leaf Radix Angelicae Pubescentis spends the assay method of middle volatile ingredient, comprises the following steps:
1) sample comminution: take the flower of decomposite leaf Radix Angelicae Pubescentis, is ground into medicinal powder (crossing 200 mesh sieves)；
2) headspace sampling: weigh above-mentioned medicinal powder 0.2000g, is directly placed into 20ml ml headspace bottle and sealing is placed in sample
Dish.Sample bottle heating-up temperature is 130 DEG C, and equilibration time is 65min；Take sample bottle headspace gas 1mL sample introduction and enter GC-MS system
System, quantitative loop temperature 130 DEG C, transmission line temperature 140 DEG C；
3) GC-MS system separation detection: separate through gas chromatogram and enter Mass Spectrometer Method.
Wherein, GC conditions: HP-5 capillary tube column type elasticity chromatographic column (0.25 μ m 250 μ m 30m)；Carrier gas:
High-purity helium, high pure nitrogen；Post flow 1.0ml min-1；Use split sampling, split ratio 10: 1；Injector temperature is 260
℃；Solvent time delay is 3.5min.Temperature programming condition: initial temperature is 50 DEG C (keeping 2min), with 2 DEG C of min-1Speed liter
Warm to 100 DEG C (keeping 3min), then with 4 DEG C of min-1Speed be warming up to 220 DEG C (keep 3min)；
Mass Spectrometry Conditions and analysis of volatile components step are with embodiment 1.
The total ion current figure of decomposite leaf Radix Angelicae Pubescentis flower volatile ingredient is shown in Fig. 4 respectively.Decomposite leaf Radix Angelicae Pubescentis flower volatile ingredient is divided into out
48 kinds of materials, 6 kinds of content of material near or above 4%, wherein o-isopropyl benzene 16.881%, γ-terpinene 15.290%, different
Terpinene 14.808%, β-caryophyllene 5.523%, trimethylbenzene methanol 4.358%, (E)-(3,3-dimethyleyelohexane subunit)-
Acetaldehyde 3.613%, accounts for more than the 60% of volatile ingredient.
Above-described embodiment can not be considered as limiting the scope of application of the present invention, and protection scope of the present invention is by enclosing
Claims are limited, and any change on the basis of the claims in the present invention is all protection scope of the present invention.
Claims (10)
1. the assay method of a Tibetan medicine material decomposite leaf Radix Angelicae Pubescentis volatile ingredient, it is characterised in that: the method comprises the following steps:
1) sample comminution: take decomposite leaf Radix Angelicae Pubescentis and need measurement site, be ground into medicinal powder；
2) headspace sampling: by above-mentioned medicinal powder, is directly placed into ml headspace bottle and sealing is placed in specimen disc.Sample bottle heating balance
After, take sample bottle headspace gas sample introduction by quantitative loop and enter GC-MS system；
3) GC-MS system separation detection: separate and enter Mass Spectrometer Method through gas chromatogram and obtain GC-MS data.
4) analysis of volatile components.
The assay method of a kind of Tibetan medicine material decomposite leaf Radix Angelicae Pubescentis volatile ingredient the most as claimed in claim 1, it is characterised in that: step
1) described medicinal powder is through 200-400 mesh sieve.
The assay method of a kind of Tibetan medicine material decomposite leaf Radix Angelicae Pubescentis volatile ingredient the most as claimed in claim 1, it is characterised in that: step
2) sample bottle heating equilibrium condition in described headspace sampling: sample bottle heating-up temperature is 60-200 DEG C, and equilibration time is 10-
120min；Quantitative loop sampling condition: quantitative loop temperature 80-180 DEG C, transmission line temperature 100-180 DEG C.
The assay method of a kind of Tibetan medicine material decomposite leaf Radix Angelicae Pubescentis volatile ingredient the most as claimed in claim 3, it is characterised in that: described
Sample bottle heating equilibrium condition: sample bottle heating-up temperature is 100 DEG C, and equilibration time is 40min.
The assay method of a kind of Tibetan medicine material decomposite leaf Radix Angelicae Pubescentis volatile ingredient the most as claimed in claim 3, it is characterised in that: described
Quantitative loop sampling condition: quantitative loop temperature 120 DEG C, transmission line temperature 140 DEG C.
The assay method of a kind of Tibetan medicine material decomposite leaf Radix Angelicae Pubescentis volatile ingredient the most as claimed in claim 1, it is characterised in that: step
3) GC conditions in described GC-MS system separation detection: HP-5 capillary tube column type elasticity chromatographic column；Carrier gas: high-purity helium,
Purity >=99.999%；High pure nitrogen, purity >=99.999%；Post flow 1.0ml min-1；Split sampling, injector temperature
For 200-300 DEG C；Solvent time delay is 3.5min.Temperature programming.
The assay method of a kind of Tibetan medicine material decomposite leaf Radix Angelicae Pubescentis volatile ingredient the most as claimed in claim 6, it is characterised in that: described
Injector temperature is 260 DEG C.
The assay method of a kind of Tibetan medicine material decomposite leaf Radix Angelicae Pubescentis volatile ingredient the most as claimed in claim 6, it is characterised in that: described
Temperature programming condition: initial temperature is 50 DEG C, keeps 2min；With 2 DEG C of min-1Speed be warming up to 100 DEG C, keep 3min；Again
With 4 DEG C of min-1Speed be warming up to 220 DEG C, keep 3min.
The assay method of a kind of Tibetan medicine material decomposite leaf Radix Angelicae Pubescentis volatile ingredient the most as claimed in claim 1, it is characterised in that: step
3) Mass Spectrometry Conditions of described GC-MS system separation detection: EI ion source, electron energy 70eV；Ion source temperature 230 DEG C；Transmission
Line temperature is 280 DEG C；Level Four bar temperature is 150 DEG C；Full scan pattern；Sweep limits: m/z 50～500.
The assay method of a kind of Tibetan medicine material decomposite leaf Radix Angelicae Pubescentis volatile ingredient the most as claimed in claim 1, it is characterised in that: step
Rapid 4) described analysis of volatile components: GC-MS data acquisition data from gas chromatography processing system, measures with areas of peak normalization method
The most each component percentage contents；Each peak in total ion current figure is obtained mass spectrum after scanning of the mass spectrum, passes through
NIST11.L mass spectrometric data system retrieval, determines volatile ingredient.
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| CN106900347A (en) * | 2017-05-09 | 2017-06-30 | 西藏藏医学院 | A kind of cultural method of high altitude localities decomposite leaf levisticum |
| CN109100431A (en) * | 2017-12-27 | 2018-12-28 | 天津中新药业集团股份有限公司达仁堂制药厂 | A kind of effective substance research method of palace of the Qing Dynasty Shoutao pills |
| CN110455964A (en) * | 2019-10-14 | 2019-11-15 | 江西中医药大学 | The analysis of Coumarins ingredient and identification method in decomposite leaf Radix Angelicae Pubescentis alcohol extract |
| CN111157654A (en) * | 2020-01-14 | 2020-05-15 | 贵州民族大学 | Method for extracting and analyzing components of fraxinus chinensis leaf volatile oil |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106900347A (en) * | 2017-05-09 | 2017-06-30 | 西藏藏医学院 | A kind of cultural method of high altitude localities decomposite leaf levisticum |
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| CN109100431B (en) * | 2017-12-27 | 2021-08-10 | 天津中新药业集团股份有限公司达仁堂制药厂 | Basic research method of drug effect substances of Qinggong Shoutao pills |
| CN110455964A (en) * | 2019-10-14 | 2019-11-15 | 江西中医药大学 | The analysis of Coumarins ingredient and identification method in decomposite leaf Radix Angelicae Pubescentis alcohol extract |
| CN111157654A (en) * | 2020-01-14 | 2020-05-15 | 贵州民族大学 | Method for extracting and analyzing components of fraxinus chinensis leaf volatile oil |
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