CN104155401B - Method for detecting contents of three kinds of fatty acids in royal jelly - Google Patents
Method for detecting contents of three kinds of fatty acids in royal jelly Download PDFInfo
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- CN104155401B CN104155401B CN201410417420.XA CN201410417420A CN104155401B CN 104155401 B CN104155401 B CN 104155401B CN 201410417420 A CN201410417420 A CN 201410417420A CN 104155401 B CN104155401 B CN 104155401B
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Abstract
The invention provides a method for detecting the contents of three kinds of fatty acids in royal jelly, wherein the three kinds of fatty acids comprise 3-hydroxy decanoic acid, 10-hydroxy decanoic acid and sebacic acid, and the contents of 3-hydroxy decanoic acid, 10-hydroxy decanoic acid and sebacic acid are detected by a gas chromatography method. Chromatographic conditions provided by the invention can make chromatographic peaks better separated, and the method is simple and convenient to operate, accurate and fast, high in sensitivity and good in reproducibility. Moreover, through the effective ingredient contents, the quality of the royal jelly is understood, and a new index is provided for royal jelly quality standards.
Description
Technical field
The invention belongs to food quality control method, relate to the detection method of Lac regis apis effective ingredient, particularly to queen bee
3-hydroxydecanoic acid, 10-hydroxydecanoic acid and the detection method of three kinds of content of fatty acid of decanedioic acid in slurry.
Background technology
Lac regis apis (royal jelly) is the hypopharyngeal gland (subpharyngeal gland) of the nurture worker bee of 5～15 ages in days
That secrete with mandibular gland (mandibular gland), in order to feed worker bee, the slurry of drone larva within queen bee and 3 ages in days
Matter.Color is creamy white or faint yellow.Its abnormal smells from the patient and mouthfeel are mainly tart flavour and acid.The chemical composition of Lac regis apis is the most multiple
Miscellaneous, containing protein, polypeptide, carbohydrate, fatty acid, vitamin, mineral, acid etc., wherein, lipid accounts for Lac regis apis dry weight
8% ~ 19%, be one of most important composition in Lac regis apis, wherein free fatty accounts for more than the 80% ~ 90% of lipid, is queen bee
Starch the material base of many biological functions such as antibacterial, immunomodulating, antitumor.
At present, 10-HAD (10-is focused primarily upon for the detection method of fatty acid composition in Lac regis apis
HDA), the reliable quantitative detecting method to other fatty acid compositions is lacked.3-hydroxydecanoic acid, 10-hydroxydecanoic acid and decanedioic acid
It is all functional fatty acid important in Lac regis apis, but the detection method research the most simply qualitative detection to these fatty acids,
Lack easy, effectively, quantitative detecting method accurately.Therefore, the method for quantitatively determining of these three fatty acid in Lac regis apis is set up
The improving further of quality control system of Lac regis apis there is great meaning.
Summary of the invention
It is an object of the invention to provide the detection method of three kinds of content of fatty acid in a kind of Lac regis apis, described three kinds of fat
Acid is respectively 3-hydroxydecanoic acid, 10-hydroxydecanoic acid and decanedioic acid,
In the Lac regis apis that the present invention provides, 3-hydroxydecanoic acid, 10-hydroxydecanoic acid and the detection method of decanedioic acid content, pass through
Following steps realize:
(1) with methyl parahydroxybenzoate, 3-hydroxydecanoic acid, 10-hydroxydecanoic acid and decanedioic acid as reference substance, make certain
The methyl parahydroxybenzoate of content, 3-hydroxydecanoic acid, 10-hydroxydecanoic acid and the solution of decanedioic acid, silylation derives, passes through
Its collection of illustrative plates of gas Chromatographic Determination, with methyl parahydroxybenzoate as internal standard substance, by methyl parahydroxybenzoate and 3-hydroxydecanoic acid,
The ratio of the ratio of the characteristic absorption peak area of 10-hydroxydecanoic acid and decanedioic acid and the sample size of reference substance draws standard curve；
(2) by Lac regis apis solubilizer supersound process to be measured, filtering to get filtrate, silylation derives, and prepares test sample；
(3) the gas chromatogram collection of illustrative plates of the test sample that determination step (2) prepares under the chromatographic condition identical with step (1),
And calculate the characteristic absorption peak peak area of methyl parahydroxybenzoate, 3-hydroxydecanoic acid, 10-hydroxydecanoic acid and decanedioic acid respectively,
The standard curve drawn according to step (1), add standard substance quality and weigh the quality of Lac regis apis and obtain 3-in Lac regis apis to be measured
Hydroxydecanoic acid, 10-hydroxydecanoic acid and the content of decanedioic acid.
Above-mentioned steps (1) dissolves methyl parahydroxybenzoate, 3-hydroxydecanoic acid, 10-hydroxydecanoic acid with 80% ~ 100% ethanol
With decanedioic acid reference substance, making methyl parahydroxybenzoate concentration is 0.1 mg/ml ~ 0.15 mg/ml, 3-hydroxydecanoic acid concentration
Be 0.004 mg/ml ~ 0.05 mg/ml, 10-hydroxydecanoic acid concentration be 0.013 mg/ml ~ 0.14 mg/ml and decanedioic acid concentration
It is the reference substance solution of 0.0015 mg/ml ~ 0.025 mg/ml, draws about 1 ml reference substance solution, use membrane filtration, wave
Dry solvent, then dissolve with 1 ~ 3 ml absolute ether, draw about 1 ml diethyl ether solution, use membrane filtration, volatilize solvent afterwards, add
Enter 300 μ l ~ 500 μ l pure pyridines and 80 μ l ~ 120 μ l BSTFA+TMS(99:1), 50 ° of C ~ 70 ° C water-baths 30 minutes ~ 60 points
Clock, then uses gas chromatographic detection.
It is 0.5 mg/ml ~ 0.75 that above-mentioned steps (2) uses 80% ~ 100% ethanol to make methyl parahydroxybenzoate concentration
The inner mark solution of mg/ml, weighs about 0.5 g Lac regis apis, is placed in volumetric flask, add 100 μ l ~ 1000 μ l 0.01mol/l ~
0.03 mol/l hydrochloric acid, vibration dissolving Lac regis apis, the inner mark solution of the accurate 3ml ~ 7ml of absorption adds volumetric flask, with 80% ~ 100%
Ethanol dilution, to scale, ultrasonic 15 minutes ~ 30 minutes, makes solution to be measured, draws about 1 ml solution to be measured, uses filter membrane mistake
Filter, volatilizes solvent, then dissolves with 1 ml ~ 3 ml absolute ether, draw 1 ml diethyl ether solution, use membrane filtration, volatilize molten afterwards
Agent, adds 300 μ l ~ 500 μ l pure pyridines and 80 μ l ~ 120 μ l BSTFA+TMS(99:1), 50 ° of C ~ 70 ° C water-baths 30 minutes
~ 60 minutes, then use gas chromatographic detection.
Use gas chromatography in above-mentioned steps (1) and step (3) is Capillary Column GC.
In above-mentioned steps (1) and step (3), the chromatographic condition of employing gas chromatogram is: use split sampling；Use (5%-
Phenyl)-methyl polysiloxane is the capillary chromatographic column of coating, carrier gas is nitrogen；Detector is fid detector.Gas chromatogram
Injector temperature be 250 ° of C, split ratio is 1:10～1:30, sample size 1 μ l；Post 50 ° of C of case temperature programming initial temperature, protect
Hold 5 minutes, then rise to 300 ° of C with 5 ° of C/ minute speed；Detector temperature is 330 ° of C；Used (5%-phenyl)-methyl
Polysiloxanes be the capillary chromatographic column of coating be Rtx-5 post, column length 30 m, internal diameter 0.25 mm, thick coating 0.25 μm.
It is a further object to provide described method in Lac regis apis to 3-hydroxydecanoic acid, 10-hydroxydecanoic acid and
The content of decanedioic acid be measured in application.
The present invention uses gas chromatography to enter the content of 3-hydroxydecanoic acid, 10-hydroxydecanoic acid and decanedioic acid in Lac regis apis
Row measures, and the chromatographic condition provided can make chromatographic peak preferably be separated, easy and simple to handle, accurate quick, and susceptiveness is high,
Favorable reproducibility.And understood the quality of Lac regis apis by the content of these effective ingredient, provide for Lac regis apis quality standard
New index.
Accompanying drawing explanation
Fig. 1 is the 3-hydroxydecanoic acid standard curve that experimental example 1 obtains.
Fig. 2 is the 10-hydroxydecanoic acid standard curve that experimental example 1 obtains.
Fig. 3 is the decanedioic acid standard curve that experimental example 1 obtains.
Specific implementation method
The present invention is further described in conjunction with the accompanying drawings and embodiments.
The methodological study of 3 kinds of fatty acid composition assays in embodiment 1 Lac regis apis
1. instrument and experimental drug
Instrument: gas chromatograph (GC 2010, Shimadzu Corp), automatic sampler (AOC-20s), FID detects
Device, GC solution work station, balance (precision 0.1mg, BS 124S, Sai Duolisi group of Germany).
Reagent: standard substance: 10-hydroxydecanoic acid (10-HDAA), 3-hydroxydecanoic acid (3-HDAA), decanedioic acid, is purchased from
Sigma company；
BSTFA+TMS(99:1) (Sigma company)；
Pyridine (Sigma company)；
Hydrogen, nitrogen, air (Hangzhou Jin Gong special gas company limited)；
Methanol (chromatographically pure, Merck company)；
Ethanol (analytical pure, Chemical Reagent Co., Ltd., Sinopharm Group)；
Absolute ether (analytical pure, Chemical Reagent Co., Ltd., Sinopharm Group)；
Hydrochloric acid (analytical pure, Chemical Reagent Co., Ltd., Sinopharm Group)；
Methyl parahydroxybenzoate (analytical pure, Chemical Reagent Co., Ltd., Sinopharm Group)；
Lac regis apis gathers from Pinghu, Zhejiang Province kind bee farm, and experimental water is ultra-pure water.
2. chromatography condition
Chromatographic column: Rtx-5, (30 m, 0.25 mmID, 0.25 μm)；Injector temperature: 250 C, sample size: 1 uL,
Split ratio: 1:20；；Post case thermograde: 50 C keep 5 min, 5 C/min to rise to 300 C, 300 C and keep 5
Min, flow rate of carrier gas: 1.0 mL/min；Detector temperature: 330 C.Methyl parahydroxybenzoate, 3-hydroxyl last of the ten Heavenly stems with this understanding
Acid, 10-hydroxydecanoic acid and decanedioic acid are good with other Component seperation in sample.
3. blank assay
Take pyridine and BSTFA+TMS mixing, water-bath 30 minutes, as blank reagent, use gas chromatographic detection, to hydroxyl
During the reservation identical with decanedioic acid reference substance of yl benzoic acid methyl ester reference substance, 3-hydroxydecanoic acid reference substance, 10-hydroxydecanoic acid reference substance
Between without absworption peak.
Weighing 0.5g Lac regis apis, be placed in 25ml volumetric flask, add 200 μ l 0.01 mol/l hydrochloric acid, honeybee is dissolved in vibration
Royal jelly, uses dehydrated alcohol to be diluted to scale, ultrasonic 15 minutes, makes solution to be measured, draw 1 ml solution to be measured, use filter membrane
Filter, volatilize solvent, then with about 1.5 ml ether dissolution, take 1 ml diethyl ether solution, use membrane filtration, volatilize solvent, add
Enter 400 μ l pyridines and 100 μ l BSTFA+TMS(99:1), 60 ° of C water-baths 30 minutes, then use gas chromatographic detection, right
Without absworption peak at the identical retention time of methyl hydroxybenzoate reference substance.
Represent that the absworption peak of target substance will not be disturbed by impurity.
4. linear relationship is investigated
Weigh 0.1625 g methyl parahydroxybenzoate, add dehydrated alcohol and be transferred in 250 mL volumetric flasks, by nothing
Water-ethanol is diluted to scale, makes inner mark solution.Precision weigh 0.0134 g 10-HDAA, 0.0049 g 3-HDAA and
0.0020 g decanedioic acid, is transferred to 50 mL volumetric flasks after adding anhydrous alcohol solution, is diluted to scale with dehydrated alcohol, shakes up,
As mixed mark mother solution.Accurate 0.5,1,2,3,4,5 mL mixed mark mother solution of drawing, in 10 mL volumetric flasks, adds 2 mL inner mark solutions
After be settled to scale.Methyl parahydroxybenzoate, 3-hydroxydecanoic acid, 10-hydroxydecanoic acid and the last of the ten Heavenly stems two is measured by above-mentioned chromatographic condition
The absworption peak area of acid, with measured matter and internal standard substance peak area ratio as abscissa, with concentration ratio as vertical coordinate, draws standard
Curve.The results are shown in Table 1-table 3.
。
5. precision and repeated experiment
Randomly selecting a Lac regis apis sample, independent extraction 6 times, make 6 independent sample, then enter according to the method described above
Row gas Chromatographic Determination, more therefrom take a sample and continuously repeat sample introduction 4 times, calculate content, seek relative standard deviation RSD.
Randomly select a Lac regis apis sample, prepare according to the method described above and treat test sample, after completing to prepare the same day, 1 day, 2
After it, after 3 days, 5 days laggard row gas Chromatographic Determination, calculate content, seek relative standard deviation RSD.The results are shown in Table 4-table 6.
6. determination of recovery rates
Use sample-adding absorption method, weigh about 0.5g Lac regis apis sample, measure 3-hydroxydecanoic acid, 10-according to preceding method
Hydroxydecanoic acid and the content of decanedioic acid, weigh 3 parts again from same Lac regis apis sample, accurate adds 3-hydroxydecanoic acid, 10-hydroxyl last of the ten Heavenly stems
Acid and decanedioic acid standard substance, measure 3-hydroxydecanoic acid, 10-hydroxydecanoic acid and the content of decanedioic acid according to preceding method, then than
Relatively.Result shows, this method has the preferable response rate.
7. the assay of 3 kinds of fatty acids in Lac regis apis
1) prepared by standard curve:
With anhydrous alcohol solution methyl parahydroxybenzoate, 3-hydroxydecanoic acid, 10-hydroxydecanoic acid and decanedioic acid reference substance,
Make the inner mark solution that methyl parahydroxybenzoate concentration is 0.65 mg/ml, 3-hydroxydecanoic acid concentration be 0.098 mg/ml,
The reference substance solution that 10-hydroxydecanoic acid concentration is 0.268 mg/ml and decanedioic acid concentration is 0.04 mg/ml, accurate absorption 0.5
Ml, 1 ml, 2 ml, 3 ml, 4 ml and 5 ml reference substance solution, to 10 ml volumetric flasks, are drawn 2 ml inner mark solutions in precision and are added
Entering volumetric flask, be diluted to scale with dehydrated alcohol, mixing is made standard curve solution, is taken 1ml standard curve solution filter membrane, will
Ethanol volatilizes, and with 1.5 ml ether dissolutions, takes 1 ml filter membrane, is volatilized by ether, adds 400 μ l pyridine and 100 μ
LBSTFA, 60 C water-baths 30 minutes, then go up gas chromatographic detection, draw standard according to content and chromatographic absorption peak result bent
Line.
2) prepared by Lac regis apis product to be tested:
The inner mark solution using dehydrated alcohol configuration methyl parahydroxybenzoate concentration to be 0.65 mg/ml, weighs 0.5 g
Lac regis apis, is placed in 25 ml volumetric flasks, adds 200 μ l 0.01mol/l hydrochloric acid, and Lac regis apis, accurate absorption 5 ml are dissolved in vibration
Inner mark solution adds volumetric flask, is diluted to scale with dehydrated alcohol, ultrasonic 15 minutes, makes solution to be measured, takes 1 ml to be measured molten
Liquid, uses membrane filtration, volatilizes solvent, with 1.5 ml ether dissolutions, takes 1 ml diethyl ether solution, uses membrane filtration, volatilize molten
Agent, adds 400 μ l pyridines and 100 μ l BSTFA+TMS(99:1), 60 C water-baths 30 minutes, then use gas chromatogram inspection
Survey, according to chromatographic absorption peak and standard curve, obtain three kinds of content of fatty acid in sample.
3) chromatographic condition:
Its chromatographic condition is: using split sampling, injector temperature is 250 C, and split ratio is 1:20, sample size 1 μ l；
Using (5%-phenyl)-methyl polysiloxane is the capillary chromatographic column of coating, and carrier gas is nitrogen, the initial temperature of post case temperature programming
Spend 50 C, keep 5 minutes, then rise to 300 C with 5 C/ minute speed；Detector is fid detector, and detector temperature is
330ºC。
Measurement result is shown in Table 8.
Claims (2)
1. a detection method for three kinds of content of fatty acid in Lac regis apis, described fatty acid is 3-hydroxydecanoic acid, 10-hydroxydecanoic acid
And decanedioic acid, it is characterised in that realized by following steps:
(1) with methyl parahydroxybenzoate, 3-hydroxydecanoic acid, 10-hydroxydecanoic acid and decanedioic acid as reference substance, certain content is made
Methyl parahydroxybenzoate, 3-hydroxydecanoic acid, 10-hydroxydecanoic acid and the solution of decanedioic acid, silylation derive, pass through gas phase
Its collection of illustrative plates of chromatographic determination, with methyl parahydroxybenzoate as internal standard substance, by methyl parahydroxybenzoate and 3-hydroxydecanoic acid, 10-
The ratio of the ratio of the characteristic absorption peak area of hydroxydecanoic acid and decanedioic acid and the sample size of reference substance draws standard curve；
(2) by Lac regis apis solubilizer supersound process to be measured, filtering to get filtrate, silylation derives, and prepares test sample；
(3) the gas chromatogram collection of illustrative plates of the test sample that determination step (2) prepares under the chromatographic condition identical with step (1), and point
Do not calculate the characteristic absorption peak peak area of methyl parahydroxybenzoate, 3-hydroxydecanoic acid, 10-hydroxydecanoic acid and decanedioic acid, according to
Standard curve that step (1) is drawn, add internal standard quality and weigh the quality of Lac regis apis and obtain the 3-hydroxyl last of the ten Heavenly stems in Lac regis apis to be measured
Acid, 10-hydroxydecanoic acid and the content of decanedioic acid；
Wherein step (1) dissolves methyl parahydroxybenzoate, 3-hydroxydecanoic acid, 10-hydroxydecanoic acid and the last of the ten Heavenly stems with 80% ~ 100% ethanol
Diacid reference substance, making methyl parahydroxybenzoate concentration is that 0.1 mg/ml ~ 0.15 mg/ml, 3-hydroxydecanoic acid concentration is
0.004 mg/ml ~ 0.05 mg/ml, 10-hydroxydecanoic acid concentration is 0.013 mg/ml ~ 0.14 mg/ml and decanedioic acid concentration is
The reference substance solution of 0.0015 mg/ml ~ 0.025 mg/ml, draws reference substance solution, uses membrane filtration, volatilizes solvent, then
With absolute ether dissolve, draw diethyl ether solution, use membrane filtration, volatilize solvent afterwards, add 300 μ l ~ 500 μ l pure pyridines and
The mixed solution of BSTFA+TMS, the volume of described mixed solution is 80 μ l ~ 120 μ l, 50 ° of C ~ 70 ° C water-baths 30 minutes ~ 60
Minute, then use gas chromatographic detection；
It is the interior of 0.5 mg/ml ~ 0.75 mg/ml that step (2) uses 80% ~ 100% ethanol to make methyl parahydroxybenzoate concentration
Mark solution, weighs 0.5 g Lac regis apis, is placed in volumetric flask, add 100 μ l 0.01mol/l ~ 0.03, μ l ~ 1000 mol/l salt
Acid, vibration is dissolved Lac regis apis, is drawn the inner mark solution addition volumetric flask of 3ml ~ 7ml, with 80% ~ 100% ethanol dilution to scale, super
Sound 15 minutes ~ 30 minutes, makes solution to be measured, draws solution to be measured, uses membrane filtration, volatilizes solvent, more molten with absolute ether
Solve, draw diethyl ether solution, use membrane filtration, volatilize solvent afterwards, add 300 μ l ~ 500 μ l pure pyridine and BSTFA+TMS
Mixed solution, the volume of described mixed solution is 80 μ l ~ 120 μ l, 50 ° of C ~ 70 ° C water-baths 30 minutes ~ 60 minutes, then
Use gas chromatographic detection；
Use gas chromatography in step (1) and step (3) is Capillary Column GC；The chromatographic condition of gas chromatogram
It is: use split sampling；Using (5%-phenyl)-methyl polysiloxane is the capillary chromatographic column of coating, and carrier gas is nitrogen；Inspection
Survey device is fid detector；The injector temperature of gas chromatogram is 250 ° of C, and split ratio is 1:10～1:30, sample size 1 μ l；Post
50 ° of C of case temperature programming initial temperature, keep 5 minutes, then rise to 300 ° of C with 5 ° of C/ minute speed；Detector temperature is
330°C；The capillary chromatographic column being used (5%-phenyl)-methyl polysiloxane to be coating is Rtx-5 post, and column length 30 m is interior
Footpath 0.25 mm, thick coating 0.25 μm.
The detection method of three kinds of content of fatty acid 3-in detection Lac regis apis in a kind of Lac regis apis the most according to claim 1
Application in hydroxydecanoic acid, 10-hydroxydecanoic acid and three kinds of fatty acids of decanedioic acid.
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| CN104569270B (en) * | 2015-01-09 | 2016-04-13 | 中国农业科学院蜜蜂研究所 | A kind of method analyzing volatile ingredient in separate sources royal jelly |
| JP6808737B2 (en) * | 2016-08-18 | 2021-01-06 | 株式会社山田養蜂場本社 | Composition for improving female alopecia |
| CN114002172B (en) * | 2021-11-05 | 2023-01-24 | 浙江大学 | Method for visually evaluating quality of royal jelly |
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