同位素稀释-超高效液相色谱串联质谱法测定卫生用品中的氯霉素

Detection of chloramphenicol in the mucosa of hygienic product by liquid chromatography tandem mass spectrometry with isotope dilution

目的:建立同位素稀释-超高效液相色谱串联质谱法测定卫生用品中氯霉素的快速测定方法。方法:样品中氯霉素用甲醇提取后,在ACQUITY UPLCTMBEH SHELD RP18色谱柱(2.1×100 mm,粒径1.7μm)中分离,以水-乙腈做流动相,超高效液相色谱在5 min内完成分离,采用负离子扫描,MRM模式定量分析。使用氯霉素—D5为内标,有效克服了样品基质和样品前处理过程所产生的影响。结果:氯霉素的最低检出限(LOD)为0.05 mg/kg。在10 ng/ml～500 ng/ml的线性范围内,相关系数r为0.999,阴性样品三水平加标平均回收率分别为:90.8%、95.5%和98.6%、日内6次测定相对标准偏差≤4.77%。结论:方法灵敏度高、操作简单、定量准确、选择性好,为皮肤黏膜卫生用品中氯霉素检测的理想方法。

Objective：To establish a ultro –LC-MS method for quantification of chloramphenicol in hygienic product.Methods： The samples were extracted using methanol and the analyses were separated on ACQUITY UPLCTM BEH SHELD RP18 column（2.1×100 mm,1.7 μm）using water-acetonitrile as mobile phase for elution.The quantitative analysis was operated by electro spray ionization mass spectrometry under the negative mode using multiple reaction monitoring（MRM）.To overcome the influence of the impurity in sample by adding chloramphenicol-D5 as internal standard.Results： The detection limit was 0.05 mg/kg.The linear calibration curves were obtained in the range of 10 ng/ml^500 ng/ml with correlation coefficient of 0.999.The average recoveries at three spiked concentration levels were 90.8%,95.5% and 98.6% with the relative standard deviations less than 4.77%.Conclusion： The method was sensitive,simple,accurate and selective and suitable for the determination of chloramphenicol in hygienic products.