CN107462654A - A kind of method that aliphatic acid forms in auxiliary esterification gas chromatography measure polyoxyethylene sorbitan monoleate using heat - Google Patents
A kind of method that aliphatic acid forms in auxiliary esterification gas chromatography measure polyoxyethylene sorbitan monoleate using heat Download PDFInfo
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- CN107462654A CN107462654A CN201710609482.4A CN201710609482A CN107462654A CN 107462654 A CN107462654 A CN 107462654A CN 201710609482 A CN201710609482 A CN 201710609482A CN 107462654 A CN107462654 A CN 107462654A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention provides the method that aliphatic acid in a kind of auxiliary esterification gas chromatography measure polyoxyethylene sorbitan monoleate using heat forms, and chromatographic separation condition, heat auxiliary esterification condition etc. are optimized on this basis；The present invention establishes the global analysis scheme for the heat auxiliary esterification gas chromatography that aliphatic acid in polyoxyethylene sorbitan monoleate forms；Determine the aliphatic acid composition of the polyoxyethylene sorbitan monoleate sample of 6 kinds of different purities；Compared with prior art, of the invention without complicated sample pretreatment process, the heat auxiliary esterification gas chromatography of exploitation is easy to operate, environmentally friendly, being capable of effectively save analysis time, simplified experimental procedure；The method that the present invention develops is applicable to analyze the aliphatic acid composition of other poly yamanashi esters materials, and the monitoring to excipient substance has very profound significance.
Description
(1) technical field
The method that aliphatic acid forms in polyoxyethylene sorbitan monoleate is determined the present invention relates to a kind of, more particularly to a kind of heat auxiliary methyl esters
The method that aliphatic acid forms in change-gas chromatography measure polyoxyethylene sorbitan monoleate.
(2) background technology
The Sorbitan Oleate of polyoxyethylene 20 that polyoxyethylene sorbitan monoleate system Sorbitan Oleate and ethylene oxide polymerization form, it is a kind of
Nonionic surface active agent, there is high surface-active, be widely used in eating frequently as emulsifying agent, solubilizer and stabilizer
Product, cosmetics and medicine etc..
With deepening continuously for Recent study, the polyoxyethylene sorbitan monoleate in medicament is relevant with adverse reaction caused by clinic.
The quality of regulation polyoxyethylene sorbitan monoleate is mainly controlled from the following aspects in version Chinese Pharmacopoeia in 2015：(1) polysorbate
The impurity residual quantity such as ethylene glycol, diethylene glycol (DEG), oxirane, dioxane in 80；(2) peroxide value of polyoxyethylene sorbitan monoleate；(3) gather
The aliphatic acid composition of sorb ester 80.
In the fatty peracid forming composition of version Chinese Pharmacopoeia regulation polyoxyethylene sorbitan monoleate in 2010, oleic acid content must not be less than
58.0%.With the continuous intensification of internationalizationof of China degree, in order to mutually be integrated with European Union and Unite States Standard, traditional Chinese medicines in versions in 2015
Allusion quotation regulation is further to the contents of other aliphatic acid to be limited in addition to oleic acid content must not be less than 58.0%, including meat
Myristic acid, palmitic acid, palmitoleic acid, stearic acid, linoleic acid and linolenic content cannot be greater than 5.0% respectively, 16.0%,
8.0%th, 6.0%, 18.0% and 4.0%.
Mainly there are gas chromatography and liquid chromatography currently for the aliphatic acid composition measuring method of polyoxyethylene sorbitan monoleate.Medicine
Aliphatic acid is carried out by esterification processing using the method that boron trifluoride methanol is heated to reflux in allusion quotation, then determines polyoxyethylene sorbitan monoleate
Aliphatic acid forms.This method sample pre-treatments step is complicated, and time-consuming, consumes a large amount of organic solvents.Report is using high in document
Effect liquid phase chromatogram-EFI fog detector and high performance liquid chromatography-tandem mass form to the aliphatic acid in polyoxyethylene sorbitan monoleate to be carried out
Analysis, but still need using sample-pretreating methods such as saponification, extractions, while the instrument and equipment used is costly, it is unfavorable
In the popularization and popularization of method.
Heat auxiliary derivatization-gas chromatographic technique be develop rapidly in recent years be used for organic acid, alcohols, phenols and amine
Deng the effective ways of species analysis.This method adds sample and derivatization reagent such as TMAH (TMAH) etc. simultaneously
It is directly injected into after cracker or mixing in gas chromatographic sample introduction mouth, the carboxyl, hydroxyl, amino groups in object are at high temperature
Reacted with derivatization reagent moment, generate corresponding ester derivative and gas chromatography system is brought into by carrier gas immediately and separated
Analysis, excessive derivatization reagent then resolve into alcohols and amine, flow out chromatographic column with carrier gas.This method is without cumbersome time-consuming
Pre-treatment step, simple to operate, quantitative accurate, high sensitivity, in the quick analysis of the complex sample with polar group compound
In play more and more important effect.
Therefore the present invention intends developing a kind of detection method simple to operate, analyze speed is fast, the degree of accuracy is high, for poly- sorb
The measure that aliphatic acid forms in ester 80.
(3) content of the invention
It is an object of the invention to provide a kind of esterification product using gas chromatography to aliphatic acid in polyoxyethylene sorbitan monoleate
The method of qualitative and quantitative analysis is carried out, and optimizes chromatographic separation condition, heat auxiliary esterification condition etc. on this basis；This
Invention establishes the global analysis scheme for heat auxiliary esterification-gas chromatography that aliphatic acid in polyoxyethylene sorbitan monoleate forms；Measure
The aliphatic acid composition of the polyoxyethylene sorbitan monoleate samples of 6 kinds of different purities.
The technical solution adopted by the present invention is as follows：
A kind of method formed using aliphatic acid in heat auxiliary esterification-gas chromatography measure polyoxyethylene sorbitan monoleate, it is described
Method comprises the following steps：
(1) following fatty acid methyl ester standard items are accurately weighed：Methyl myristate, methyl hexadecanoate, Methyl palmitoleinate,
Methyl stearate, methyl oleate, methyl linoleate and methyl linolenate, standard solution is configured to methanol dissolving；
Recommend in the standard solution, the concentration of each fatty acid methyl ester standard items is 0.1mg/mL；
(2) standard solution (recommending the μ L of sample size 1) prepared in aspiration step (1) is placed in specimen cup, by specimen cup
It is put into cracker, cracker is placed at gas chromatograph injection port, when cracking furnace temperature reaches 250-400 DEG C (preferably 300
DEG C) when sample introduction, with gas chromatograph on-line checking, the gas chromatogram of fatty acid methyl ester standard items is obtained, as qualitative analysis
Foundation；
The GC conditions：Chromatographic column is RB-5 (30m × 0.25mm × 0.25 μm), and heating schedule is initial temperature 50
DEG C, 200 DEG C are raised to 10 DEG C/min speed, keeps 10min, 250 DEG C is raised to 5 DEG C/min speed, keeps 10min；Injection port
Temperature is 300 DEG C, detector FID, and temperature is 300 DEG C, split ratio 30:1；Carrier gas is nitrogen, flow velocity 1.0mL/min；
Cracker condition：Crack furnace temperature：250-400 DEG C (preferably 300 DEG C)；Cracker and gas chromatograph interface temperature
300℃；
(3) accurately weighed polyoxyethylene sorbitan monoleate sample, sample solution is configured to methanol dissolving, then by sample solution and derivative
Change reagent mixing, ultrasound is uniformly mixed so as to obtain solution to be measured；
Recommend in the sample solution, the concentration of polyoxyethylene sorbitan monoleate sample is 10mg/mL；
The derivatization reagent is the methanol solution of 0.2mol/L trimethyl hydroxide sulphur；
Recommend the sample solution and derivatization reagent by volume 1：2 mixing；
(4) take gained solution to be measured (recommending the μ L of sample size 3) in step (3) to be mounted in specimen cup, specimen cup is put into and split
Solve in device, cracker is placed at gas chromatograph injection port, when cracking furnace temperature reaches 250-400 DEG C (preferably 300 DEG C)
Sample introduction, with gas chromatograph on-line checking, testing conditions are identical with step (2), obtain the gas phase color of polyoxyethylene sorbitan monoleate sample
The contrast of fatty acid methyl ester standard items spectrogram is carried out qualitative in spectrogram, with step (1), is quantified using chromatographic peak area normalization method,
And then obtain the measurement result that aliphatic acid forms in polyoxyethylene sorbitan monoleate sample.
The invention has the advantages that：
1. compared with prior art, the present invention is without complicated sample pretreatment process.Heat auxiliary esterification-gas of exploitation
Phase chromatography is easy to operate, environmentally friendly, being capable of effectively save analysis time, simplified experimental procedure.
2. the method that the present invention develops is applicable to analyze the fat of other poly yamanashi esters materials (such as polysorbate 20)
Acid composition, the monitoring to excipient substance have very profound significance.
(4) illustrate
Fig. 1：The gas chromatogram of seven kinds of fatty acid methyl ester standard items；
Fig. 2：Pharmaceutical grade polyoxyethylene sorbitan monoleate gained gas chromatogram after heat aids in esterification；
Fig. 3：The pure polyoxyethylene sorbitan monoleate of chemistry gained gas chromatogram after heat auxiliary methylates；
Mark in Fig. 1~3 for：1- methyl myristates, 2- Methyl palmitoleinates, 3- methyl hexadecanoates, 4- leukotrienes
Methyl esters, 5- methyl linoleates, 6- methyl oleates, 7- methyl stearates.
(5) embodiment
Below by specific embodiment, the present invention is further illustrated, but protection scope of the present invention is not limited in
This.
The selection of the input mode of embodiment 1
Polyoxyethylene sorbitan monoleate sample 0.1g is taken, it is accurately weighed, it is placed in 10mL volumetric flask, with methanol constant volume, is store after shaking up
Refrigerator is stored in, as sample solution.
Input mode one：The 1 above-mentioned sample solutions of μ L and derivatization reagent 0.2mol/L trimethyl hydroxide sulphur are drawn respectively
The μ L of methanol solution 2 are placed in specimen cup.
Input mode two：Take the 50 above-mentioned sample solutions of μ L and derivatization reagent 0.2mol/L trimethyl hydroxide sulphur methanol molten
The μ L of liquid 100 are placed in ultrasound mixing in 0.5mL sample cells, take the solution after 3 μ L mixings to be mounted in specimen cup.
Specimen cup equipped with sample is put into cracker, cracker is placed at gas chromatograph injection port, works as cracking
Sample introduction when furnace temperature reaches 300 DEG C, with gas chromatograph on-line checking, obtain the gas phase color of the derivatization product of polyoxyethylene sorbitan monoleate
Spectrogram；It is qualitative with the contrast progress of standard items spectrogram, quantified using chromatographic peak area normalization method.
GC conditions：Chromatographic column is RB-5 (30m × 0.25mm × 0.25 μm), and heating schedule is 50 DEG C of initial temperature, with
10 DEG C/min speed is raised to 200 DEG C, keeps 10min, is raised to 250 DEG C with 5 DEG C/min speed, keeps 10min；Injector temperature is
300 DEG C, detector FID, temperature is 300 DEG C, split ratio 30:1；Carrier gas is nitrogen, flow velocity 1.0mL/min；
Cracker condition：Crack furnace temperature：300℃；300 DEG C of cracker and gas chromatograph interface temperature.
The reappearance RSD values of each content of fatty acid of the gained of input mode one are between 5.0%-46.6%, and input mode
Two reappearance RSD values are between 0.3%-9.1%.Therefore selection is analyzed using input mode two.
Embodiment 2 cracks the selection of furnace temperature
The chromatogram that cracking furnace temperature is polyoxyethylene sorbitan monoleate esterification product at 300 DEG C, 350 DEG C and 400 DEG C has been investigated respectively
Response, it is as a result basically identical.Therefore selection uses cracking furnace temperature to be analyzed for 300 DEG C.
The methodology of embodiment 3 is examined or check
Methylated using heat auxiliary-gas chromatography analyzed the polyoxyethylene sorbitan monoleate sample of 6 kinds of different purities, we
The reappearance RSD values of method are less than 9.1%.
The analysis that aliphatic acid forms in 43 kinds of pharmaceutical grade polyoxyethylene sorbitan monoleate samples of embodiment
Polyoxyethylene sorbitan monoleate sample 0.1g is taken, it is accurately weighed, it is placed in 10mL volumetric flask, with methanol constant volume, is store after shaking up
Refrigerator is stored in, as sample solution.Take the 50 above-mentioned sample solutions of μ L and derivatization reagent 0.2mol/L trimethyl hydroxide sulphur first
The μ L of alcoholic solution 100 are placed in ultrasound mixing in 0.5mL sample cells, take the solution after 3 μ L mixings to be mounted in specimen cup.Sample will be housed
Specimen cup be put into cracker, cracker is placed at gas chromatograph injection port, when crack furnace temperature reach 300 DEG C when enter
Sample, with gas chromatograph on-line checking, testing conditions are in the same manner as in Example 1, obtain the derivatization product of polyoxyethylene sorbitan monoleate
Gas chromatogram；It is qualitative with the contrast progress of standard items spectrogram, quantified using chromatographic peak area normalization method.Sample detection result is equal
Meet version Chinese Pharmacopoeia regulation in 2015, specific data are as follows：
Numerical value in bracket is reappearance RSD values (n=5)
The analysis that aliphatic acid forms in the non-pharmaceutical grade polyoxyethylene sorbitan monoleate sample of 53 kinds of embodiment
Polyoxyethylene sorbitan monoleate sample 0.1g is taken, it is accurately weighed, it is placed in 10mL volumetric flask, with methanol constant volume, is store after shaking up
Refrigerator is stored in, as sample solution.Take the 50 above-mentioned sample solutions of μ L and derivatization reagent 0.2mol/L trimethyl hydroxide sulphur first
The μ L of alcoholic solution 100 are placed in ultrasound mixing in 0.5mL sample cells, take the solution after 3 μ L mixings to be mounted in specimen cup.Sample will be housed
Specimen cup be put into cracker, cracker is placed at gas chromatograph injection port, when crack furnace temperature reach 300 DEG C when enter
Sample, with gas chromatograph on-line checking, testing conditions are in the same manner as in Example 1, obtain the derivatization product of polyoxyethylene sorbitan monoleate
Gas chromatogram；It is qualitative with the contrast progress of standard items spectrogram, quantified using chromatographic peak area normalization method.Sample detection result is equal
Version Chinese Pharmacopoeia regulation in 2015 is not met, specific data are as follows：
Numerical value in bracket is reappearance RSD values (n=5)
Comparative example
Aliphatic acid according to polyoxyethylene sorbitan monoleate is determined in Chinese Pharmacopoeia version in 2015 forms：This product about 0.1g is taken, precision claims
It is fixed, put in 50mL conical flasks, add 2% sodium hydrate methanol solution 2mL, put in 65 DEG C of water-baths and be heated to reflux 30min, let cool, add
14% boron trifluoride methanol solution 2mL, is heated to reflux 30min, lets cool in a water bath, adds normal heptane 4mL, continues to add in a water bath
Heat backflow 5 minutes, lets cool, adds saturated nacl aqueous solution 10mL, shakes, and standing makes layering, takes upper liquid, is washed with water 3 times, often
Secondary 4mL, upper liquid is after anhydrous sodium sulfate drying, as need testing solution.1 μ L need testing solutions are taken to be mounted in specimen cup.Will
Specimen cup equipped with sample is put into cracker, and cracker is placed at gas chromatograph injection port, when cracking furnace temperature reaches
Sample introduction at 300 DEG C, with gas chromatograph on-line checking, obtain the gas chromatogram of the methylate of polyoxyethylene sorbitan monoleate；With mark
Quasi- product spectrogram contrast progress is qualitative, is quantified using chromatographic peak area normalization method.
The result that aliphatic acid forms in 3 kinds of pharmaceutical grade polyoxyethylene sorbitan monoleate samples is analyzed using Chinese Pharmacopoeia version in 2015
Numerical value in bracket is reappearance RSD values (n=5)
The result that aliphatic acid forms in 3 kinds of non-pharmaceutical grade polyoxyethylene sorbitan monoleate samples is analyzed using Chinese Pharmacopoeia version in 2015
Numerical value in bracket is reappearance RSD values (n=5).
Claims (7)
1. a kind of method formed using aliphatic acid in heat auxiliary esterification-gas chromatography measure polyoxyethylene sorbitan monoleate, its feature
It is, the described method comprises the following steps：
(1) following fatty acid methyl ester standard items are accurately weighed：Methyl myristate, methyl hexadecanoate, Methyl palmitoleinate, tristearin
Sour methyl esters, methyl oleate, methyl linoleate and methyl linolenate, standard solution is configured to methanol dissolving；
(2) standard solution prepared in aspiration step (1) is placed in specimen cup, and specimen cup is put into cracker, will be cracked
Device is placed at gas chromatograph injection port, the sample introduction when cracking furnace temperature and reaching 250-400 DEG C, is examined online with gas chromatograph
Survey, obtain the gas chromatogram of fatty acid methyl ester standard items, the foundation as qualitative analysis；
The GC conditions：Chromatographic column is RB-5, and heating schedule is 50 DEG C of initial temperature, and 200 DEG C are raised to 10 DEG C/min speed,
10min is kept, 250 DEG C is raised to 5 DEG C/min speed, keeps 10min；Injector temperature is 300 DEG C, detector FID, temperature
For 300 DEG C, split ratio 30:1；Carrier gas is nitrogen, flow velocity 1.0mL/min；
Cracker condition：Crack furnace temperature：250-400℃；300 DEG C of cracker and gas chromatograph interface temperature；
(3) accurately weighed polyoxyethylene sorbitan monoleate sample, sample solution is configured to methanol dissolving, then sample solution and derivatization is tried
Agent mixes, and ultrasound is uniformly mixed so as to obtain solution to be measured；
The derivatization reagent is the methanol solution of 0.2mol/L trimethyl hydroxide sulphur；
(4) take gained solution to be measured in step (3) to be mounted in specimen cup, specimen cup is put into cracker, cracker is placed in
At gas chromatograph injection port, the sample introduction when cracking furnace temperature and reaching 250-400 DEG C, with gas chromatograph on-line checking, detection
Condition is identical with step (2), obtains the gas chromatogram of polyoxyethylene sorbitan monoleate sample, with fatty acid methyl ester standard in step (1)
The contrast progress of product spectrogram is qualitative, is quantified using chromatographic peak area normalization method, and then obtains aliphatic acid in polyoxyethylene sorbitan monoleate sample
The measurement result of composition.
2. as claimed in claim 1 formed using aliphatic acid in heat auxiliary esterification-gas chromatography measure polyoxyethylene sorbitan monoleate
Method, it is characterised in that in step (1) described standard solution, the concentration of each fatty acid methyl ester standard items is 0.1mg/
mL。
3. as claimed in claim 1 formed using aliphatic acid in heat auxiliary esterification-gas chromatography measure polyoxyethylene sorbitan monoleate
Method, it is characterised in that standard solution sample size described in step (2) is 1 μ L.
4. as claimed in claim 1 formed using aliphatic acid in heat auxiliary esterification-gas chromatography measure polyoxyethylene sorbitan monoleate
Method, it is characterised in that in step (2) or (4), it is described cracking furnace temperature be 300 DEG C.
5. as claimed in claim 1 formed using aliphatic acid in heat auxiliary esterification-gas chromatography measure polyoxyethylene sorbitan monoleate
Method, it is characterised in that in step (3) described sample solution, the concentration of polyoxyethylene sorbitan monoleate sample is 10mg/mL.
6. as claimed in claim 1 formed using aliphatic acid in heat auxiliary esterification-gas chromatography measure polyoxyethylene sorbitan monoleate
Method, it is characterised in that in step (3), the sample solution and derivatization reagent by volume 1：2 mixing.
7. as claimed in claim 1 formed using aliphatic acid in heat auxiliary esterification-gas chromatography measure polyoxyethylene sorbitan monoleate
Method, it is characterised in that solution sample size to be measured described in step (4) is 3 μ L.
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| CN110095533A (en) * | 2019-03-13 | 2019-08-06 | 江苏知原药业有限公司 | The improvement of Sorbitan Stearate (sorbester p18) fatty acid composition measuring method |
| CN110609100A (en) * | 2019-09-26 | 2019-12-24 | 上海美农生物科技股份有限公司 | Method for simultaneously detecting 6 organic acids in compound acidifier by gas chromatography |
| CN110967419A (en) * | 2019-11-06 | 2020-04-07 | 浙江工业大学 | Determination of fatty acid content of different forms in polysorbate 80 by heat-assisted online derivatization gas chromatography |
| CN111208247A (en) * | 2020-01-08 | 2020-05-29 | 浙江工业大学 | Method for measuring content of gamma-hydroxybutyric acid in human hair by online heat-assisted methylation-gas chromatography mass spectrometry |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109613153A (en) * | 2018-12-27 | 2019-04-12 | 国家海洋局第三海洋研究所 | Method that is a kind of while detecting suitable anti-palmitoleic acid |
| CN110095533A (en) * | 2019-03-13 | 2019-08-06 | 江苏知原药业有限公司 | The improvement of Sorbitan Stearate (sorbester p18) fatty acid composition measuring method |
| CN110609100A (en) * | 2019-09-26 | 2019-12-24 | 上海美农生物科技股份有限公司 | Method for simultaneously detecting 6 organic acids in compound acidifier by gas chromatography |
| CN110967419A (en) * | 2019-11-06 | 2020-04-07 | 浙江工业大学 | Determination of fatty acid content of different forms in polysorbate 80 by heat-assisted online derivatization gas chromatography |
| CN111208247A (en) * | 2020-01-08 | 2020-05-29 | 浙江工业大学 | Method for measuring content of gamma-hydroxybutyric acid in human hair by online heat-assisted methylation-gas chromatography mass spectrometry |
| CN113049727A (en) * | 2021-03-08 | 2021-06-29 | 哈尔滨瀚邦医疗科技有限公司 | Method for detecting polysorbate 80 content |
| CN113049727B (en) * | 2021-03-08 | 2024-04-26 | 哈尔滨瀚邦医疗科技有限公司 | Method for detecting content of polysorbate 80 |
| CN114137113A (en) * | 2021-11-26 | 2022-03-04 | 重庆伊诺生化制品有限公司 | Method for detecting content of fatty acid in polysaccharide |
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Application publication date: 20171212 |