A method for determining the content of 11 kinds of illegally added drugs in Chinese veterinary medicine powder

A technology for illegally adding and veterinary drugs, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of low sensitivity, poor accuracy, complicated operation, etc., and achieve the effect of simple pretreatment and good recovery rate

Active Publication Date: 2017-08-11
SHANDONG ANALYSIS & TEST CENT
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Regarding the detection methods of illegally added drugs in traditional Chinese veterinary drugs, there are currently thin-layer chromatography, infrared spectroscopy, capillary electrophoresis, atomic absorption method, liquid chromatography, etc., but the above methods have problems such as cumbersome operation, low sensitivity or poor accuracy.

Method used

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  • A method for determining the content of 11 kinds of illegally added drugs in Chinese veterinary medicine powder
  • A method for determining the content of 11 kinds of illegally added drugs in Chinese veterinary medicine powder
  • A method for determining the content of 11 kinds of illegally added drugs in Chinese veterinary medicine powder

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Embodiment 1

[0046] 1. Optimization of chromatographic conditions

[0047] In this study, a 2.1×150mm, 5μm C18 chromatographic column was selected to ensure the effective separation of 11 illegally added drugs in a relatively short period of time. The experiment compares the influence of methanol-water and acetonitrile-water system as the mobile phase on the separation effect of 11 illegally added drugs. The results show that the selectivity of the test compound in the acetonitrile-water mobile phase is better than that of methanol-water system and due to the The polarity difference is large, and the experiment adopts the gradient elution method to obtain the ideal chromatographic separation effect, and the single operation time is only 10min.

[0048] 2. Optimization of mass spectrometry conditions

[0049] Table 1 Optimized mass spectrometry conditions for 11 illegally added drugs (the ones with * are quantified ions)

[0050]

[0051] Using the flow injection method, each compound ...

Embodiment 2

[0063] Actual sample analysis

[0064] Pulsatilla powder, Zhili powder, Qingwenbaidu powder, Yinqiao powder, Chuanxinlian powder, Huanglian Jiedu powder, Fuzheng Jiedu powder, Xiaoshi Pingwei powder, Jingfang Baidu powder, Gongying powder, Qingfeizhike powder, Wupi powder San, Qibu San, Sangju San and other 35 commercially available Chinese veterinary medicine powders were detected by HPLC-MS / MS (see the total ion chromatogram of the samples in Figure 12 and Figure 13 As shown), the test results showed that none of the 11 types of illegally added drugs were detected in the veterinary medicine powder to be tested.

[0065] in conclusion

[0066] In this paper, high performance liquid chromatography tandem mass spectrometry was used to establish an analytical method for 11 illegally added drugs in Chinese veterinary medicine powder. The method is simple, fast, sensitive, specific, and reproducible. It can simultaneously determine 11 illegally added drugs, realizing its high...

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Abstract

The invention discloses a method for measuring content of 11 illegally added medicaments in veterinary drug powder. The method comprises the following steps of (1) pre-treating veterinary drug powder to be measured by adopting an organic solvent ultrasonic extraction method, wherein an organic solvent is methanol-water, and a volume ratio of methanol to water is (0.9-1.1):(0.9-1.1); (2) detecting olaquindox, ribavirin, amantadine, rimantadine, dexamethasone, chloramphenicol, diethylstilbestrol, furaltodone, nitrofurantoin, nitrofural and furazolidone in extract by adopting liquid chromatography-tandem mass spectrometry. According to the method, a sample can be simply pre-treated by adopting methanol / water (50+50) as an extraction reagent for ultrasonic extraction, and can be loaded on a machine for detection after passing through a filter membrane, and a recovery rate is high; the method is lower in detection limit, a detection limit of the olaquindox, ribavirin, amantadine, rimantadine, dexamethasone, chloramphenicol, furaltodone and furazolidone is 50mu g / kg, and a detection limit of the nitrofurantoin, nitrofural and diethylstilbestrol is 100mu g / kg.

Description

technical field [0001] The invention relates to a method for determining the content of 11 kinds of illegally added medicines in Chinese veterinary medicine powder. Background technique [0002] Traditional Chinese veterinary medicine has the advantages of relatively small toxic and side effects, no residue or less residue in animal-derived foods, and less resistance to drugs. Its products are increasingly valued by livestock and poultry farmers. As a key target for preventing and treating diseases and promoting animal growth. At present, some lawbreakers take advantage of the loopholes in the supervision of veterinary drugs to illegally add chemical drugs with definite curative effects and widely used to make Chinese veterinary drugs with moderate curative effects quick-acting and other advantages. These chemical components are transmitted through the food chain and eventually cause serious harm to human health. The detection of illegally added chemical drugs in traditiona...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 王晓利赵汝松苑金鹏王珊珊陈相峰李磊赵金宁凡盛王超
Owner SHANDONG ANALYSIS & TEST CENT
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