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目的建立猪肉中氯霉素残留量检测的超高效液相色谱-四级杆-静电场轨道阱高分辨质谱法(UPLC-Q Extractive MS)。方法样品经乙酸乙酯提取,加入正己烷净化后,采用BEH C18柱(2.0 mm×50 mm,2.1μm)色谱柱分离,以甲醇-5 mmol/L乙酸铵为流动相,梯度洗脱,Q Excative MS电喷雾电离负离子模式检测。在t-SIM扫描模式下,通过理论精确质量数与所测得的精确质量数之间的匹配度、目标化合物的元素组成、保留时间、同位素化合物丰度比定性,以氯霉素-D5为内标定量。结果氯霉素在1.0μg/L~50.0μg/L线性关系良好,相关系数为0.999 0,方法检出限为0.2μg/kg,定量限为0.6μg/kg,加标回收率为77.9%~85.2%,相对标准偏差(RSD)<3%。结论本方法简便快捷,选择性好,灵敏度高,重现性好,适用于猪肉中氯霉素残留的快速分析测定。
Objective To establish an ultra performance liquid chromatography-quadrupole column-electrostatic field orbit-well high resolution mass spectrometry (UPLC-Q Extractive MS) for the determination of chloramphenicol residues in pork. Methods The samples were extracted with ethyl acetate and purified with n-hexane. The samples were separated on a BEH C18 column (2.0 mm × 50 mm, 2.1 μm) using methanol-5 mmol / L ammonium acetate as mobile phase and gradient elution. Q Excative MS Electrospray ionization negative ion mode detection. In the t-SIM scan mode, through the match between the theoretical accurate mass number and the measured exact mass number, the elemental composition of the target compound, the retention time, the abundance ratio of isotope compound qualitative analysis, chloramphenicol-D5 Internal standard quantification. Results The linearity of chloramphenicol in the range of 1.0μg / L ~ 50.0μg / L was good, the correlation coefficient was 0.999 0, the detection limit was 0.2μg / kg, the limit of quantification was 0.6μg / kg, the recovery was 77.9% 85.2%, relative standard deviation (RSD) <3%. Conclusion The method is simple, rapid, selective, sensitive and reproducible. It is suitable for the rapid determination of chloramphenicol residues in pork.