液相色谱-串联质谱法测定血清中硫酸头孢噻利浓度

目的：建立一种灵敏、可靠的检测血清中硫酸头孢噻利含量的高效液相色谱-串联质谱法。方法：血清样品经酸化甲醇蛋白沉淀后，采用ExtendC18柱（250mm×4．6mm，5μm）0．02mol·L^-1乙酸铵-甲醇（65：35）为流动相，头孢唑啉为内标，应用高效液相色谱／大气压化学电离串联质谱法在多反应监测模式（MRM）下测定，硫酸头孢噻利和内标的定量离子对分别为m/z 523→396和m／z455→323。结果：硫酸头孢噻利的回收率在94．0％-101．9％之间，硫酸头孢噻利在2．0～1000．0μg·L^-1范围内呈良好线性，日内RSD〈9．2％，日间RSD〈10．6％，定量检出限为2．0μg·L^-1。结论：本方法简便、灵敏、干扰少、特异性好，可用于硫酸头孢噻利的临床药动学研究及临床特殊人群的血药浓度测定。

Determination of Cefoselis Sulsate in Human Serum by High-performance Liquid Chromatography Coupled with Tandem Mass Spectrometry

Objective： To develop a sensitive and accurate method for the determination of cefoselis sulsate in human serum by high-performance liquid chromatography coupled with tandem mass spectrometry （HPLC-MS/MS）. Method： After cefoselis sulsate in human serum was extracted by protein precipitation with acidic methanol ,the separation was performed on an Extend C18 column（ 250 mm× 4.6 mm, 5 μm）, the mobile phase consisted of 0.02 mol·L ^-1 acetic ammonium-methanol （65/： 35 ）. Detection was carried by a positive atmospheric pressure chemical ionization （APCI） in the multiple reaction monitoring （MRM） mode with the transitions of m/ z 523→396 and m/z 455→323 for cefoselis sulsate and cefazolin （an internal standard） , respectively. Result： Calibration curve was linear within the range of 2.0-1000.0 μg·L^-1 ,the recoveries were from 94.0% -101.9% ,the intra-day RSD were less than 9.2% ,and the inter-day RSD were less than 10.6%. The limit of quantitation was 2.0μg·L^-1 for eefoselis sulsate in human serum. Condusion： This method is simple, sensitive, little interferential and good specificity for pharmacokinetic studies and the determination of cefoselis sulsate in human serum for patients.