| 摘要: |
| 建立氟苯尼考注射液中非法添加的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 ~ 100 μg/mL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。 |
| 关键词: 超高效液相色谱-四级杆-飞行时间质谱 高效液相色谱法 氟苯尼考注射液 二氧丙嗪 |
| DOI： |
| 投稿时间：2017-02-03修订日期：2017-10-16 |
| 基金项目: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） |
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| Determination of Dioxopromethazine Illegally Adultered into Florfenicol Injection |
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| (Zhejiang Provincial Supervisory Institute of Veterinary Drug and Feedstuff) |
| Abstract: |
| 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. |
| Key words: UHPLC-Q/TOF MS HPLC florfenicol injection dioxopromethazine |
