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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 rapid method for the determination of chloramphenicol in sanitary products by isotope dilution-ultra performance liquid chromatography-tandem mass spectrometry. METHODS: Chloramphenicol was extracted with methanol and separated on an ACQUITY UPLC TMBEH SHELD RP18 column (2.1 × 100 mm, particle size 1.7 μm). The mobile phase consisted of water and acetonitrile. After 5 min Complete separation, the use of negative ion scan, MRM mode quantitative analysis. The use of chloramphenicol-D5 as an internal standard effectively overcomes the effects of sample matrix and sample pretreatment. Results: The detection limit of chloramphenicol (LOD) was 0.05 mg / kg. In the linear range of 10 ng / ml to 500 ng / ml, the correlation coefficient r was 0.999. The average recoveries of the three samples in the negative samples were 90.8%, 95.5% and 98.6%, respectively. The relative standard deviations 4.77%. Conclusion: The method has high sensitivity, simple operation, accurate quantitation and good selectivity. It is an ideal method for the detection of chloramphenicol in skin and mucous membrane hygiene articles.