摘要
建立氟苯尼考注射液中非法添加二氧丙嗪的检测方法。对1批氟苯尼考注射液照《中国兽药典》2010版HPLC法进行含量测定时,发现未知物质峰。采用超高效液相色谱-四级杆-飞行时间质谱(UHPLC-Q/TOF MS)对该批检品进行筛查,发现该添加物疑似二氧丙嗪,并采用高效液相色谱-二极管阵列检测法(HPLC-DAD)对二氧丙嗪进行定性和定量检测。结果显示,高效液相色谱法二氧丙嗪在1~100μg/m L浓度范围内的线性良好(r=1.0000),平均回收率为99.5%,RSD为0.3%。本方法专属性强,灵敏度高,重现性好,适用于氟苯尼考注射液中非法添加二氧丙嗪的检测。
To establish a method for determination of dioxopromethazine illegally added in florfenicol injection. In the course of content determination of 1 batch florfenicol injection with the method of HPLC according to the Chinese Veterinary Pharmacopoeia 2010, a suspicious compound peak was found. The suspicious compound was found by quadrupole time-of-flight tandem mass spectrometry （UHPLC-Q/TOF MS）, then confirmation and content determination were completed by high performance liquid chromatography-diode array detector （ HPLC- DAD） . The suspicious compound in this sample was identified as dioxopromethethazine. The results showed that there was a good linear correlation between the peak areas and the concentrations of dioxopromethazine at the range of 1- 100 μg/mL（r= 1.0000）. The average recovery was 99.5% with RSD of 0.3% by HPLC. The method is convenient, reliable and accurate. It was suitable for detection of dioxopromethazine illegally adulterated in florfenicol injection.
出处
《中国兽药杂志》
北大核心
2017年第11期44-50,共7页
Chinese Journal of Veterinary Drug
基金
公益性行业(农业)科研专项(201203023-4)
浙江省"三农六方"科技协作专项(中兽药注射剂中非法添加物控制技术研究与风险监测)
