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目的建立一种快速、灵敏、可靠的测定全血中氯霉素含量的分散固相萃取-同位素稀释-超快速液相色谱-串联质谱的分析方法。方法全血样品经乙腈沉淀蛋白后,利用自制的氨基功能化Fe3O4磁性高分子复合微粒(EDA-MPs)吸附剂进行净化,采用Eclipse Plus C18柱(100 mm×2.1 mm,2.2μm),以乙腈-水为流动相进行梯度洗脱,在电喷雾负离子多反应监测(MRM)模式下,以氯霉素-D5为内标,采用同位素稀释法定量检测。结果氯霉素在质量浓度0.05~10.0μg·L-1时具有良好的线性关系(r=0.999 5),定量检出限(RSN>10)为0.05μg·L-1,方法的提取回收率98.8%~101.5%,低、中、高3种加标浓度质控样品的日内RSDs<6.0%,日间RSDs<8.0%。结论建立的方法准确性好、操作简便、灵敏度高,符合生物样品分析要求。
Objective To establish a rapid, sensitive and reliable method for the determination of chloramphenicol in whole blood by dispersive solid-phase extraction-isotope dilution-ultra-fast liquid chromatography-tandem mass spectrometry. Methods Whole blood samples were precipitated with acetonitrile and purified with homemade amino-functionalized Fe3O4 magnetic polymer composite particles (EDA-MPs) using Eclipse Plus C18 column (100 mm × 2.1 mm, 2.2 μm) - water as the mobile phase gradient elution. In electrospray negative ion MRM mode, chloramphenicol-D5 was used as internal standard, and the amount of chloramphenicol-D5 was determined by isotope dilution method. Results Chloramphenicol had a good linear relationship (r = 0.999 5) with a mass concentration of 0.05 ~ 10.0 μg · L-1 and a detection limit (RSN> 10) of 0.05 μg · L-1. 98.8% ~ 101.5%, RSDs <6.0%, daytime RSDs <8.0% for low, medium and high quality control samples. Conclusion The established method has good accuracy, simple operation, high sensitivity and meets the requirements of biological sample analysis.