Improved method for measuring fatty acid composition of sorbitan monostearate
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A determination method and fatty acid technology, which can be used in measurement devices, instruments, scientific instruments, etc., and can solve the problem of high error rate
Inactive Publication Date: 2019-08-06
JIANGSU SEMPOLL PHARMA
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There is a certain error between this method and the actual situation, and the error rate is relatively high, which needs to be improved
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Embodiment 1
[0016] Accurately weigh 0.6000g and 0.4000g of standard palmitic acid and stearic acid, and react with an appropriate amount of raw material sorbitan to obtain a sample of Span 60 through esterification, take 0.1g of sample 1, and test sample 1 according to the following method:
[0017] Take 0.1g of this product, put it in a 50ml round bottom flask, add 4ml of 0.5mol / L potassium hydroxide methanol solution, heat and reflux in a water bath at 65°C for 30 minutes, let it cool, add 5ml of 14% boron trifluoride methanol solution, Heat and reflux in a 65°C water bath for 5 minutes, let cool, add 5ml of n-hexane, continue to heat and reflux in a 65°C water bath for 5 minutes, let cool, add 10ml of saturated sodium chloride solution, shake well, let stand to separate layers, and take the upper layer Liquid, dried over anhydrous sodium sulfate; test according to gas chromatography (general rule 0521). Use polyethylene glycol as the fixed liquid capillary column as the chromatographic...
Embodiment 2
[0023] Test sample 2 (with embodiment 1) as follows:
[0024] Chinese Pharmacopoeia (2015 edition) method:
[0025] Take 0.1g of this product, put it in a 50ml round bottom flask, add 4ml of 0.5mol / L potassium hydroxide methanol solution, heat and reflux in a water bath at 65°C for 10 minutes, let it cool, add 5ml of 14% boron trifluoride methanol solution, Heat and reflux in a water bath at 65°C for 2 minutes, let cool, add 5ml of n-hexane, continue to heat and reflux in a water bath at 65°C for 1 minute, let cool, add 10ml of saturated sodium chloride solution, shake well, let stand to separate layers, and take the upper layer Liquid, dried over anhydrous sodium sulfate; test according to gas chromatography (general rule 0521). Use polyethylene glycol as the fixed liquid capillary column as the chromatographic column, the initial temperature is 150°C, maintain for 3 minutes, increase the temperature to 220°C at a rate of 5°C per minute, and maintain for 10 minutes; the temp...
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Abstract
The invention discloses an improved method for measuring the fatty acid composition of sorbitan monostearate. The method comprises: taking a sample and placing the sample into a flask; adding a potassium hydroxide methanol solution, carrying out heating refluxing, and carrying out cooling; adding a methanol solution, carrying out heating refluxing, and carrying out cooling; adding normal hexane, and carrying out heating refluxing continuously, and carrying out cooling; adding a saturated sodium chloride solution, carrying out shaking uniformly, carrying out standing for layering, and taking supernatant fluid and carrying out anhydrous sodium sulfate drying; carrying out testing based on a gas chromatographic method; with a capillary column with polyethylene glycol as stationary liquid as achromatographic column, taking a proper amount of methyl palmitate and methyl stearate reference substances respectively and carrying out dilution to make a solution containing 1mg of methyl palmitate and 1mg of methyl stearate respectively per 1ml under conditions of keeping the feeding inlet temperature of 240 DEG C and the detector temperature of 280 DEG C; injecting the solution into a gas chromatograph and recording a chromatogram map with the separation degrees of all chromatographic peaks meeting requirements; and taking the supernatant fluid and injecting the fluid into the gas chromatograph, recording a chromatogram map, and carrying out calculation with a peak area based on an area normalization method. With the disclosed method, the error rate is low.
Description
technical field [0001] The invention relates to an improved method for determining fatty acid composition of sorbitan stearyl (Span 60). [0002] 【Background technique】 [0003] Sorbitan monostearate, also known as Span 60, S-60, is light yellow to tan waxy solid with a slight odor. Used as emulsifier and defoamer in pesticide, plastic, cosmetic, pharmaceutical, paint, textile, food and other industries. The HLB value is 4.7. [0004] Sorbitan monostearate (Span 60) is a food additive prepared by esterification of stearic acid and sorbitan as raw materials. The Ministry of Health of the People's Republic of China issued the national food safety standard on sorbitan monostearate on November 21, 2011. The current standard number is GB 19301-2010, which replaces GB 13481-2010 "National Food Safety Standard". Standard Food Additive Sorbitan Monostearate (Span 60)" (now abolished), implemented since December 21, 2011. [0005] The Chinese Pharmacopoeia (2015) recorded a method...
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