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目的建立LC-MS/MS法同时测定士的宁及其代谢物士的宁氮氧化物在大鼠血浆中的浓度。方法以盐酸麻黄碱为内标,甲醇沉淀法处理血浆样品。采用ZORBAX Eclipse XDB-C18柱(2.1 mm×150 mm,3.5μm)分离,以甲醇-10 mmol·L-1乙酸铵(用甲酸调p H=4)为流动相进行梯度洗脱,流速0.2 m L·min-1,用电喷雾离子化和正离子多离子反应监测(MRM)模式检测士的宁和士的宁氮氧化物。结果士的宁及其氮氧化物的线性范围分别为0.510~306.3 ng·m L-1和0.102~306.0 ng·m L-1,定量下限分别为0.510,0.102 ng·m L-1,日内、日间相对标准偏差(RSD)均<15%,准确度分别为(89.44±3.43)%~(97.45±6.25)%和(95.86±5.19)%~(106.41±7.43)%。结论该方法准确、灵敏、特异、简便,适用于血浆中士的宁及其代谢物士的宁氮氧化物含量的同时测定。
Objective To establish a simultaneous LC-MS / MS method for the determination of the concentration of strychnine and its metabolites in rats plasma. Methods Using ephedrine hydrochloride as internal standard, plasma samples were treated by methanol precipitation. The sample was separated on a ZORBAX Eclipse XDB-C18 column (2.1 mm × 150 mm, 3.5 μm) and eluted with 10 mmol·L -1 ammonium acetate (adjusted to formic acid p H = 4) as mobile phase at a flow rate of 0.2 m L · min-1. The strychnine and strychnine nitrogen oxides were detected by electrospray ionization and positive ion multi-ion reaction monitoring (MRM). Results The linear ranges of strychnine and its nitrogen oxides ranged from 0.510 to 306.3 ng · m L-1 and from 0.102 to 306.0 ng · m L-1, with the lower limits of quantitation of 0.510 and 0.102 ng · m L-1, respectively. The daytime relative standard deviations (RSDs) were all less than 15%, with accuracy of (89.44 ± 3.43)% ~ (97.45 ± 6.25)% and (95.86 ± 5.19)% ~ (106.41 ± 7.43)%, respectively. Conclusion The method is accurate, sensitive, specific and simple and suitable for the simultaneous determination of nifloxacin in plasma and its metabolites.