HPLC-MS/MS法同时测定人血浆中对乙酰氨基酚和布洛芬  

Simultaneous Determination of Acetaminophen and Ibuprofen in Human Plasma by HPLC-MS/MS

作　　者：马彦博 王美银 彭路路 张枢 李小川 段小群[1] MA Yan-bo;WANG Mei-yin;PENG Lu-lu;ZHANG Shu;LI Xiao-chuan;DUAN Xiao-qun(Department of Pharmacy,Guilin Medical University,Guilin 541100,China;Suzhou Xuhui Testing Co.,LTD.,Suzhou 215300,China)

机构地区：[1]桂林医学院药学院,广西桂林541100 [2]苏州旭辉检测有限公司,江苏苏州215300

出　　处：《海峡药学》2024年第8期73-77,共5页Strait Pharmaceutical Journal

基　　金：仿制药一致性评价及关键技术研究与产业化应用示范(桂科AA22096025)。

摘　　要：目的建立一种可以同时测定人血浆中对乙酰氨基酚和布洛芬的液相色谱-串联质谱法(HPLC-MS/MS)。方法选用对乙酰氨基酚-d_(3)和布洛芬-d_(3)为内标,采用甲醇蛋白沉淀法处理血浆样品。色谱柱采用ZORBAX Extend C_(18)(4.6×150 mm,3.5μm),选用梯度洗脱方式,流动相A为5 mM乙酸铵水溶液,流动相B为甲醇;采用电喷雾离子化多反应监测模式:0~3.50 min,以正离子检测对乙酰氨基酚和对乙酰氨基酚-d_(3),3.5~5.5 min,以负离子检测布洛芬和布洛芬-d_(3)。结果对乙酰氨基酚和布洛芬分别在0.0400~10.0μg·mL^(-1)、0.100~25.0μg·mL^(-1)内线性关系良好,且精密度、回收率、稳定性等考察均符合要求。结论该方法快速简便,灵敏、准确且选择性好,适用于对乙酰氨基酚和布洛芬的临床药代动力学研究。OBJECTIVE To develop a high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)for simultaneous determination of acetaminophen and ibuprofen in human plasma.METHODS Plasma samples were treated by the protein precipitation method with methanol and the internal standard was acetaminophen-d_(3) and ibuprofen-d_(3).A ZORBAX Extend C_(18)(4.6×150 mm,3.5μm)column was used for gradient elution with 5 mM ammonium acetate aqueous solution as mobile phase A and methanol as mobile phase B.Electrospray ionization multi-reaction monitoring mode was used:0-3.50 min,positive ions were used to detect acetaminophen and acetaminophen-d_(3),3.5-5.5 min,negative ions were used to detect ibuprofen and ibuprofen-d_(3).RESULTS The calibration curves of acetaminophen and ibuprofen were linear in the ranges of 0.0400-10.0μg·mL^(-1) and 0.100-25.0μg·mL^(-1),and the precision,recovery and stability investigation conforms to the requirements.CONCLUSION The method is rapid,simple,sensitive,precise and selective.It is suitable for the study of clinical pharmacokinetics of acetaminophen and ibuprofen.

关 键 词：HPLC-MS/MS 对乙酰氨基酚 布洛芬 药动学 

分 类 号：R969.1[医药卫生—药理学]