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Method for testing 3-chlorine-1, 2-propylene glycol and aliphatic ester content of 3-chlorine-1, 2-propylene glycol

A technology of propylene glycol fatty acid ester and a detection method, applied in the field of analytical chemistry, can solve the problems of high user's business ability requirements, high maintenance and use costs, limited promotion and application, etc., and achieves low price, reduced equipment investment, and easy popularization and application. Effect

Active Publication Date: 2012-07-11
湖北莱菔子科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although GC-MS is the main method currently used, this method has defects such as expensive instruments, high maintenance and use costs, deuterated standard samples as internal standards, and high requirements for users' professional capabilities, which greatly limit this method. The popularization and application of detection methods has made it empty talk to add 3-chloro-1,2-propanediol residue indicators in related products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Example 1: Weigh 2g first-grade soybean oil, dissolve it in 10mL methyl tert-butyl ether, add 20mL sodium methoxide solution for transesterification for 10min, then add 60mL hexane and 60mL NaCl-containing acetic acid solution to extract 3-chloro- 1,2-Propanediol, discard the upper organic phase; repeat extraction with 60 mL of hexane, add 0.1 mol / L sodium periodate solution to the resulting aqueous phase for oxidation reaction, where the volume of the sodium periodate solution is the resulting aqueous phase 10% of the volume, the reaction temperature is 30℃, the reaction time is 20min; Concentrate to a volume of 1mL, then add 2mL of 0.002mol / L guanine for derivatization reaction, react at 37℃ for 240min; after the reaction is completed, the volume is constant To 5mL, use the HPLC-FLD method to detect: the stationary phase is reversed-phase ODS filler, the mobile phase is methanol-water (5:95, v / v); the excitation wavelength is 260nm, the fluorescence detection wavelength...

Embodiment 2

[0035] Example 2: Weigh 2g lard, dissolve it in 10mL methyl tert-butyl ether, add 20mL sodium methoxide solution for transesterification for 10min, then add 60mL hexane and 60mL NaCl-containing acetic acid solution to extract 3-chloro-1, 2-Propanediol, discard the upper organic phase; repeat the extraction with 60 mL of hexane, add 0.05 mol / L sodium periodate solution to the resulting aqueous phase for oxidation reaction, where the volume of the sodium periodate solution is the volume of the resulting aqueous phase 40%, reaction temperature is 20℃, reaction time is 50min; concentrate to a volume of 1mL, then add 0.8mL of 0.01mol / L guanine for derivatization reaction, react at 50℃ for 120min; after completion of the reaction, dilute to 5mL, detected by HPLC-FLD method: the stationary phase is reversed-phase ODS filler, the mobile phase is acetonitrile-water (10:90, v / v); the excitation wavelength is 280nm, the fluorescence detection wavelength is 380nm; the external standard meth...

Embodiment 3

[0036] Example 3: Weigh 2g of primary rapeseed oil, dissolve it in 10mL of methyl tert-butyl ether, add 20mL of sodium methoxide solution for transesterification for 10min, then add 60mL of hexane and 60mL of acetic acid solution containing NaCl to extract 3-chloro -1,2-propanediol, discard the upper organic phase; repeat extraction with 60 mL of hexane, add 0.01mol / L sodium periodate solution to the resulting aqueous phase for oxidation reaction, where the volume of sodium periodate solution is the resulting water 80% of the phase volume, reaction temperature of 5℃, reaction time of 120min; concentration to a volume of 1mL, then add 0.5mL of 0.02mol / L adenosine for derivatization reaction, react at 100℃ for 20min; After completion, dilute the volume to 5 mL and use HPLC-FLD method to detect: the stationary phase is reversed-phase C12 packing, the mobile phase is methanol-water (15:85, v / v); the excitation wavelength is 320nm, and the fluorescence detection wavelength is 470nm; ...

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PUM

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Abstract

The invention discloses a method for testing 3-chlorine-1, 2-propylene glycol. The method comprises the steps: (1) oxidizing the 3-chlorine-1, 2-propylene glycol in a water solution into chloroacetaldehyde; (2) performing derivatization to subject the chloroacetaldehyde and a derivatization reagent to a reaction to produce substances with fluorescent effects; and (3) using a high performance liquid chromatograph-forming limit diagram (HPLC-FLD) method to perform testing, and obtaining content of 3-chlorine-1, 2-propylene glycol. Compared with an existing gas chromatography-mass spectrometer (GC-MS) method, the method is simple in operation, equipment investment is greatly reduced, an expensive deuterated master standard is not needed, the using cost is greatly reduced, and barriers are cleared for addition of testing indexes of 3-chlorine-1, 2-propylene glycol for relative products. 3-chlorine-1, 2-propylene glycol aliphatic ester is converted into 3-chlorine-1, 2-propylene glycol by ester exchange so that the aliphatic ester content of 3-chlorine-1, 2-propylene glycol is tested.

Description

Technical field [0001] The invention belongs to the field of analytical chemistry, and specifically relates to a method for detecting the content of 3-chloro-1,2-propanediol and its fatty acid ester. Background technique [0002] 3-Chloro-1,2-propanediol and its fatty acid esters are substances that are produced during food processing and are not easy to attract people's attention, but are harmful to the health of consumers. Its harm to the human body is manifested in: ① Acute and chronic toxicity of 3-chloro-1,2-propanediol: the oral half-lethal LD ​​of rats with 3-chloro-1,2-propanediol 50 It is 150mg / kg.bw. When male rats are continuously orally exposed to 3-chloro-1,2-propanediol at a dose of 1 mg / kg / day or more, sperm motility and fertility may be reduced. The dose is greater than or equal to 10-20 mg / kg / day, which can be seen Mouse sperm has significant morphological changes and epididymal damage; ②Genetic toxicity of 3-chloro-1,2-propanediol: At present, most research ins...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/89
Inventor 张维农胡志雄齐玉堂程鹏
Owner 湖北莱菔子科技有限公司
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