用HPLC-MS/MS法测定比格犬血浆中盐酸哌罗匹隆的浓度  

Determination of perospirone hydrochloride in the plasma of Beagle dogs by HPLC-MS/MS method

作　　者：庞佩汶 李威 吴丹 徐升扬 吴波 PANG Pei-wen;LI Wei;WU Dan;XU Sheng-yang;WU Bo(School of Pharmaceutical Sciences,Guangzhou Medical University,Guangzhou 511436,Guangdong Province,China)

机构地区：[1]广州医科大学药学院,广东广州511436

出　　处：《中国临床药理学杂志》2023年第13期1954-1958,共5页The Chinese Journal of Clinical Pharmacology

摘　　要：目的 建立应用液质联用(HPLC-MS/MS)技术测定比格犬血浆中盐酸哌罗匹隆的方法。方法 比格犬血浆经乙腈(含内标卡马西平)沉淀蛋白处理。色谱柱为ACQUITY UPLC BEH HILIC(2.1 mm×50 mm,1.8μm),柱温为40℃。流动相为含0.1%甲酸的水溶液和含0.1%甲酸的乙腈溶液,流速为0.4 mL·min^(-1),梯度洗脱。盐酸哌罗匹隆和卡马西平的质谱检测方式均为电喷雾正离子模式,多反应监测(MRM)。结果 盐酸哌罗匹隆在0.05~25 ng·mL^(-1)线性良好(r^(2)=0.998 7),定量下限为0.05 ng·mL^(-1);批内及批间精密度和准确度、提取回收率、稀释倍数验证和基质效应均符合性能验证要求,选择性良好,分析批次的适用性良好,基质中的稳定性良好。结论 此方法具有简便、快捷、准确、灵敏等特点,有望为盐酸哌罗匹隆治疗药物检测及其体内药代动力学分析提供理论基础。Objective To establish a method for the determination of perospirone hydrochloride in the plasma of beagle dogs by HPLC-MS/MS.Methods Beagle dog plasma were treated with acetonitrile(containing internal standard carbamazepine)to precipitate protein.The chromatography column was ACQUITY UPLC BEH HILIC(2.1 mm×50 mm,1.8μm),whose column temperature was 40℃.The mobile phase was an aqueous solution containing 0.1%formic acid and an acetonitrile solution containing 0.1%formic acid at a flow rate of 0.4 mL·min^(-1),and gradient elution.Both perospirone and carbamazepine mass spectrometry detection methods were electrospray positive ion mode,multiple reaction monitoring(MRM).Results Perospirone hydrochloride has a good linearity in the range of 0.05-25 ng·mL^(-1)(r^(2)=0.9987),and the lower limit of quantification was 0.05 ng·mL^(-1).The precision and accuracy within and between batches,extraction recovery,dilution factor verification,and matrix effect met the perfomance verification requirements,with good selectivity,good applicability for analyzing batches,and good stability in the matrix.Conclusion This method is simple,fast,accurate,and sensitive,and it's expected to provide a theoretical basis for the detection of perospirone hydrochloride therapeutic drug and its in vivo pharmacokinetic analysis.

关 键 词：盐酸哌罗匹隆 高效液相色谱-串联质谱法 比格犬 药代动力学 方法学验证 

分 类 号：R97[医药卫生—药品]