用LC-MS/MS法测定人血浆中哌柏西利的浓度  

Determination of palbociclib in human plasma by LC-MS/MS

作　　者：戴丽静 杨烨 刘威杨 何秀玲 温预关[1] DAI Li-jing;YANG Ye;LIU Wei-yang;HE Xiu-ling;WEN Yu-guan(Phase Ⅰ Clinical Laboratory of Brain Hospital Afiliated to Guangzhou Medical University,Guangzhou 510370,Guangdong Province,China;Guangzhou Medical University New Drug Creation Co.,Ltd,Guangzhou 510700,Guangdong Province,China;Phase I Clinical Research Center,The Affiliated Jiangmen Hospital of Traditional Chinese Medicine of Jinan University,Jiangmen 529000,Guangdong Province,China)

机构地区：[1]广州医科大学附属脑科医院Ⅰ期临床研究室,广东广州510370 [2]广州医大新药创制有限公司,广东广州510700 [3]暨南大学附属江门中医院I期临床研究中心,广东江门529000

出　　处：《中国临床药理学杂志》2023年第9期1326-1330,共5页The Chinese Journal of Clinical Pharmacology

基　　金：广东省卫生计生适宜推广基金资助项目(粤卫办函[2018]326号);广东省医院药学研究基金(澳美基金)资助项目(2022A22)。

摘　　要：目的建立一种可靠、灵敏、专属的LC-MS/MS法测定人血浆中哌柏西利浓度,拟应用于人体药代动力学试验生物样本的测定。方法以哌柏西利-d8为内标,用蛋白沉淀法进行血浆样本前处理,用反相色谱柱Agilent Eclipse plus C18(2.1 mm×50 mm,1.8μm),以0.1%甲酸水溶液为A流动相,0.1%甲酸乙腈为B流动相,流速为0.4 mL·min^(-1),梯度洗脱;在正离子模式下,多反应监测模式扫描检测哌柏西利m/z 448.1→m/z 380.1和哌柏西利-d8m/z 456.0→m/z 388.1。结果该方法在1~160 ng·mL^(-1)线性关系良好,定量下限为1 ng·mL^(-1),批内、批间精密度%CV在0.65%~5.23%,平均准确度偏差在-2.64%~6.13%,提取回收率%CV为1.77%。结论该方法灵敏度高,前处理简单,适用于哌柏西利药代动力学试验的血浆样本测定。Objective To establish a reliable,sensitive and exclusive LC-MS/MS method for the determination of palbociclib in human plasma to be used for determination of biological samples in human pharmacokinetic study.Methods Palbociclib-d was used as the internal standard.The plasma samples were pretreated by protein precipitation extraction.Agilent Eclipse plus C18(2.1 mm×50 mm,1.8μm)reversed-phase column was used.Aqueous containing 0.1%formic acid solution was used as A mobile phase,and acetonitrile containing 0.1%formic acid was used as B mobile phase.The flow rate was O.4 mL min-I with gradient elution;in positive ion mode,multiple reaction monitoring mode scanning was used to detect palbociclib m/z 448.1→m/z 380.1 and palbociclib-dg m/z 456.0→m/z 388.1.Results The method showed good linearity in the concentration range of 1-160 ng mL^(-1)and the lower limit of quantification was 1 ng:mL-1.The intra-batch and inter-batch%CV was within 0.65%-5.23%,and the average accuracy deviation was within-2.64%-6.13%.The extraction recovery%CV was 1.77%.Conclusion The method has high sensitivity and simple pretreatment,and is suitable for the determination1of plasma samples applicable to palbociclib pharmacokinetic trials.

关 键 词：高效液相色谱法 质谱法 哌柏西利 

分 类 号：R971[医药卫生—药品]