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目的建立快速、灵敏的液相色谱-串联质谱法测定人血浆中环酯红霉素的浓度。方法 50μL血浆样品经正己烷-二氯甲烷-异丙醇(300∶150∶15)液-液萃取后,以甲醇-5mmol·L-1醋酸铵-甲酸溶液(75∶25∶0.2)为流动相,采用Capcell Pak C18MG(2.0mm×35mm,3μm)柱分离。使用电喷雾电离源以多反应监测(MRM)方式进行正离子检测。结果测定血浆中环酯红霉素线性范围为1.00～2000ng·mL-1,定量下限为1.00ng·mL-1,灵敏度提高了20倍。日内、日间精密度(RSD)均小于9.6%,准确度(RE)在±0.9%以内。环酯红霉素和内标罗红霉素的回收率分别为80.4%和79.3%。每个样品分析时间为2.5min。结论该方法灵敏度高、选择性强、准确快速,适用于环酯红霉素片人体生物等效性研究。
OBJECTIVE To establish a rapid and sensitive liquid chromatography-tandem mass spectrometry (HPLC-tandem mass spectrometry) method for the determination of erythromycin in human plasma. Methods 50μL plasma samples were liquid-liquid extracted with n-hexane-dichloromethane-isopropanol (300:150:15) and then eluted with methanol-5mmol·L-1 ammonium acetate-formic acid solution Phase using a Capcell Pak C18 MG (2.0 mm x 35 mm, 3 μm) column. Electrospray ionization sources are used for positive ion detection in multiple reaction monitoring (MRM) mode. Results The linear range of erythromycin in the plasma ranged from 1.00 to 2000 ng · mL-1 and the limit of quantification was 1.00 ng · mL-1. The sensitivity was improved 20-fold. Day and day precision (RSD) were less than 9.6%, accuracy (RE) within ± 0.9%. The recoveries of cyclic ester erythromycin and internal standard roxithromycin were 80.4% and 79.3%, respectively. Each sample analysis time was 2.5 min. Conclusion The method is sensitive, selective, rapid and accurate and is suitable for bioequivalence study of erythromycin.