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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 materials and production methods, different types of impurities brought in also interfere with the accuracy of the analysis results

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

Embodiment 1

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

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

[0049] Preparation of the test solution: Get 1.0 g of gelatin samples (Bengbu Fengyuan Tushan Pharmaceutical Company, batch numbers 20100406M and 20120504), put it in a 20ml volumetric flask, add 10.0ml of mixed solvent, sonicate for 3.5 hours, cool to room temperature, take 1.0g ml, add 0.8ml of internal standard solution to obtain.

[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 (polyethylene glycol 20000 filled);

[0052] Chromatographic column specificati...

Embodiment 2

[0061] Embodiment 2 system suitability experiment

[0062] According to the detection method of Example 1, the reference substance solution was continuously injected 5 times, and the ratio of the peak area of ​​2-chloroethanol in the reference substance collection to the internal standard peak area was calculated, and its RSD must not be greater than 10.0%. Based on the peak of 2-chloroethanol, 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 Figure 1-5 .

[0064] Table 12-Chlorohydrin system suitability test

[0065]

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

[0067] Detection limit:

[0068] By diluting the reference substance solution, the final measured concentration of 2-chloroethanol solution is 0.03 μg / ml. The signal-to-noise ratio after injection is 3.8:1, so we dete...

Embodiment 3

[0069] Embodiment 3 specificity experiment

[0070] Because impurity 2-chloroethanol and ethylene glycol may be contained in the gelatin raw material, 2-chloroethanol and ethylene glycol are diluted with water; Collect the chromatograms after sample injection respectively, and mix the above-mentioned 3 kinds of solutions before injecting samples, and collect the chromatograms. According to the retention time of the peaks of each substance, it is shown that the method is used to detect 2-chloroethanol, and its specificity is good. See the attached picture for details Figure 7-10 .

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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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