超高效液相色谱-四级杆静电场轨道阱高分辨质 谱法测定猪肉中氯丙嗪及其代谢物
目的 建立适用于猪肉中氯丙嗪及代谢物7-羟基氯丙嗪残留的超高效液相色谱-四级杆/静电场轨道阱高分辨质谱法(ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry, UPLC-Q-Orbitrap HRMS)。方法 猪肉样品均质后, 使用添加1%乙酸的乙腈提取和去除蛋白质等杂质, 经低温高速离心后达到净化样品的目的。选用Thermo accucore RP-MS(100 mm×2.1 mm, 2.6 μm)色谱柱对待测物进行分离, 在Q Exactive高分辨质谱Full MS/dd-MS2扫描模式下采集数据进行定性定量分析。结果 2种目标物在1~200 μg/kg浓度范围内线性良好, 相关系数r2均大于0.9900。3个添加水平的平均回收率80.2%~94.2%, 精密度(relative standard deviation, RSD)均小于2%。结论 该法重现性好、灵敏度高、操作简便, 适用于猪肉中氯丙嗪及代谢物7-羟基氯丙嗪残留的定性、定量筛查。
Objective To establish a method for determination of chlorpromazine and 7-hydroxychloroprozine residues in pork by ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry (UPLC-Q-Orbitrap HRMS). Methods After homogenization of pork samples, 1% acetic acid acetonitrile was used to extract and remove impurities such as protein. The samples were purified by centrifugation at low temperature and high speed. The Thermo accucore RP-MS (100 mm×2.1 mm, 2.6 μm) chromatographic column was used to separate the analytes. Quantitative and qualitative analysis were performed on Q Exactive Full-MS/dd-MS2 scan mode. Results In the range of 1-200 μg/kg, 2 targets had good linear relationships with correlation coefficients more than 0.9900. At the 3 spiked levels, the average recoveries were 80.2%-94.2% and relative standard deviations were below 2%. Conclusion The method has good reproducibility, high sensitivity and is easy to operate, which is suitable for qualitative and quantitative determination of chlorpromazine and 7-hydroxychloroprozine residues in pork.
标题：超高效液相色谱-四级杆静电场轨道阱高分辨质 谱法测定猪肉中氯丙嗪及其代谢物
英文标题：Determination of chlorpromazine and its metabolites in pork by ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry
作者：
程建桥 沈阳化工大学
王传胜 沈阳化工大学
张峰 中国检验检疫科学研究院食品安全所
中文关键词:超高效液相色谱-四级杆/静电场轨道阱高分辨质谱法,残留,猪肉,氯丙嗪,
英文关键词:ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry,residues,pork,chlorpromazine,
发表日期：2018-03-02
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