中兽药散剂中非法添加酰胺醇类药物的检测方法研究

Study on the detection method of illegal addition of amide-alcohols in Chinese veterinary drug powder

关键词:  中兽药散剂，酰胺醇类，非法添加，高效液相色谱

Key words:  Chinese veterinary medicine powder,amide alcohol, illegal addition, HPLC

摘要:

本文建立了高效液相色谱测定中兽药散剂中甲砜霉素、氟苯尼考、氯霉素3种非法添加药物的方法。该方法采用Waters Atlantis T3 色谱柱（4.6mm×250mm，5μm），以甲醇-乙腈-水为流动相进行梯度洗脱，流速为1.0 mL/min，检测波长为224和278 nm。该方法选取4种常见中药散剂：健胃散、止痢散、球虫散、胃肠活。经验证，甲砜霉素的检测限为3g/kg、氟苯尼考及氯霉素的检测限均为4g/kg，对照溶液的线性范围为10 ~500 μg/mL，峰面积的相对标准偏差分别为0.11%、0.11%、0.13%。按外标法计算其回收率，三种药物的回收率在均在98.0%~103.0%，变异系数均在0.6%~1.6%。与传统的标准检测方法相比，本研究最终完成了几种中兽药制剂中同时检测三种酰胺醇类药物，突破了原有标准中一种药物的检测方法，提高了检测工作效率，同时该方法具有较好的灵敏度、准确度和稳定性，能够满足对三种药物常规检测的要求。在实际工作中，通过对不同类别固体兽药制剂进行实验探索验证，得出该方法具有很好的适用性，为相关检测单位的检测工作提供了一定的技术支持，提高违法添加的检出率。

Abstract:

A method for the determination of Thiamphenicol, Florfenicol and Chloramphenicol in the Chinese veterinary medicine powders by HPLC was established. Waters Atlantis T3 column (4.6 mm x 250 mm, 5 μm) was used in this method with a methanol-acetonitrile-water mobile phase, gradient elution at a flow rate of 1.0 mL/min and detection wavelengths of 224 and 278 nm. Four kinds of common Chinese medicine powders was selected: Jianwei Powder, Zhizhi Powder, Coccidial Powder and Gastrointestinal Activity. It has been verified that the detected limitation of Thiamphenicol is 3g/kg, Florfenicol and Chloramphenicol is 4g/kg. The linear range of the contrastive solution is 10 ~ 500 μg/mL, and the relative standard deviations of peak areas were 0.11%, 0.11% and 0.13%, respectively. The recoveries of the three drugs were all in the range of 98.0%~103.0% according to the external standard method, and the coefficients of variation were all in the range of 0.6%~1.6%. Compared with the traditional standard detection methods, this study finally completed the simultaneous detection of three amide alcohol drugs in several Chinese veterinary drug preparations, which broke the detection method of one drug in the original standard and improved the efficiency of detection work. The method has good sensitivity, accuracy and stability, which can adapt the requirements for routine detection of three drugs. In the actual work, it is concluded that the method has good applicability through experimental exploration and verification of different types of solid veterinary drug preparations. The method provided certain technical support for the detection work of related testing units and improved the detection rate of illegal addition.