Method for rapidly detecting 2-chloroethanol residues in gelatin

A technology of chlorohydrin and gelatin, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of time-consuming and interference with the accuracy of analysis results, etc., and achieve the goals of improving detection accuracy, shortening preparation time, saving time and operation steps Effect

Inactive Publication Date: 2016-04-27
蚌埠丰原涂山制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the existing analysis methods have the problem of taking too long
And because the samples to be tested have different raw

Method used

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  • Method for rapidly detecting 2-chloroethanol residues in gelatin
  • Method for rapidly detecting 2-chloroethanol residues in gelatin
  • Method for rapidly detecting 2-chloroethanol residues in gelatin

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0046] Example 1:

[0047] Mixed solvent: methanol-acetonitrile (25:75V / V)

[0048] Preparation of internal standard solution: take 0.250g of n-hexanol and add mixed solvent to dissolve and dilute to 50ml, take 0.5ml and add mixed solvent to dilute to 50ml, that is.

[0049] Preparation of test solution: Take 1.0 g of gelatin sample (Bengbu Fengyuan Tushan Pharmaceutical Co., Ltd., batch number 20100406M and 20120504), put it in a 20ml volumetric flask, add 10.0ml of mixed solvent, ultrasonically treat it for 3.5 hours, cool it to room temperature, take 1.0 ml, add 0.8ml of internal standard solution, and get it.

[0050] Preparation of reference solution: take 0.250g of 2-chloroethanol, add water to dilute to 50ml, take 1.0ml and add water to dilute to 100ml, then take 1.0ml and add water to dilute to 10ml, mix well, take 1.0ml, add 0.8ml of internal standard solution, that is have to.

[0051] Chromatographic column: DB-WAX (packed with polyethylene glycol 20000);

[005...

Example Embodiment

[0061] Example 2 System Applicability Experiment

[0062] According to the detection method of Example 1, the reference substance solution was continuously injected for 5 times, and the ratio of the peak area of ​​2-chloroethanol to the peak area of ​​the internal standard substance in the reference substance spectrum was calculated, and its RSD should not be greater than 10.0%. Based on the 2-chloroethanol peak, the signal-to-noise ratio shall not be less than 10:1.

[0063]The specific results are shown in Table 1, and the chromatograms are shown in the appendix. Figures 1 to 5 .

[0064] Table 12 - Applicability Test of Chloroethanol System

[0065]

[0066] The results show that the main peak in this system has no interference, the separation is good, and it meets the requirements.

[0067] Detection limit:

[0068] By diluting the reference solution, a 2-chloroethanol solution with a concentration of 0.03 μg / ml was finally measured. After injection, the signal-to-...

Example Embodiment

[0069] Example 3 Specificity Experiment

[0070] Because the gelatin raw material may contain impurities 2-chloroethanol and ethylene glycol, 2-chloroethanol and ethylene glycol are diluted with water as a solvent; the internal standard substance is diluted with a methanol-acetonitrile mixed solvent (the method of dilution is the same as in Example 1), Collect the spectrum after injecting the samples respectively, and mix the above three solutions before injecting the samples to collect the spectrum. According to the retention time of the peaks of each substance, it is explained that the method is used to detect 2-chloroethanol, and its specificity is good, and the chromatography is See attached picture for details Figures 7 to 10 .

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Abstract

The invention provides a method for rapidly detecting 2-chloroethanol residues in gelatin. The method comprises the following steps: 1) taking hexyl alcohol as an internal standard substance; 2) using a methanol-acetonitrile mixed solvent for dissolving a gelatin sample, 3) dissolving 2-chloroethanol in a methanol-acetonitrile mixed solvent, adding the internal standard solution according to volume ratio of 1:07-0.9 to obtain a product as a reference substance solution; and 4)using polyethylene glycol 20000 for filling a chromatographic column DB-WAX, preciously absorbing 1-2 [mu]l of the reference substance solution and a tested object solution for sampling, recording a chromatogram, calculating ratio of a peak area of 2-chloroethanol to the peak area of the internal standard. The provided method aims at the pollution generated during a gelatin production process for selecting the solvent. The used methanol-acetonitrile mixed solvent rapidly and effectively dissolve the gelatin sample, compared with the prior art, time and operation step can be saved; and the employed ultrasonic extraction can shorten preparation time of the tested object solution.

Description

technical field [0001] The invention belongs to the field of organic chemistry, and in particular relates to a detection method for halogenated alcohols. Background technique [0002] When gelatin raw materials are used to prepare capsules, ethylene oxide is usually used for sterilization during the production process. Ethylene oxide (EO) is a broad-spectrum low-temperature sterilant that can kill various microorganisms at room temperature, including spores. , viruses, bacteria, etc. Ethylene oxide is a highly toxic gas, which has allergenic, mutagenic and carcinogenic effects, and is easily adsorbed on many objects. Ethylene oxide reacts with chloride ions in the article to generate 2-chloroethanol (EthyleneChlorohydrin, referred to as ECH). Due to its high toxicity, the limit specified in the Pharmacopoeia is 8.8ppm, and a gas phase detection method is given . According to the Pharmacopoeia, n-hexane is used as the solvent in the pretreatment of the sample. In order to ...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 张爱文汪君洪厚林汪林
Owner 蚌埠丰原涂山制药有限公司
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