Yan Miao, Zhu Yun-Gui, Li Huan-De, Chen Ben-Mei, Ma Ning, Lei Yan-Qing, Liu Yi-Ping
Clinical Pharmacy & Pharmacology Research Institute, The Second Xiangya Hospital of Central South University, 139# Middle Renmin Road, Changsha, Hunan 410011, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2009 Oct 1;877(27):3243-7. doi: 10.1016/j.jchromb.2009.07.038. Epub 2009 Aug 7.
A sensitive and specific method using a one-step liquid-liquid extraction with dichloromethane followed by liquid chromatographic-electrospray ionization-mass spectrometric was developed and validated to determine prochlorperazine maleate in human plasma using amitriptyline hydrochloride as an internal standard. The samples were separated using a Thermo Hypersil-Hypurity C18 reversed-phase column (150mmx2.1mm i.d., 5mum). A mobile phase containing 10mM ammonium acetate (pH 3.6)-methanol-acetonitrile (27:68:5, v/v/v) was used isocratically eluting at a flow rate of 0.22ml/min. The average extraction recovery of prochlorperazine and internal standard were 81.8+/-2.2% and 79.5+/-3.7%, respectively. Prochlorperazine maleate and internal standard were measured by electrospray ion source in positive selective ion monitoring mode. The method demonstrated that good linearity ranged from 0.20 to 6.40ng/ml with r(2)=0.9989. The limit of quantification for prochlorperazine maleate in the plasma was 0.20ng/ml. The established method has been successfully applied to a bioequivalence study of two prochlorperazine maleate formulations in 18 healthy male Chinese volunteers.
建立并验证了一种灵敏且特异的方法,该方法采用二氯甲烷一步液-液萃取,随后进行液相色谱-电喷雾电离-质谱分析,以盐酸阿米替林为内标物测定人血浆中的马来酸氯丙嗪。使用Thermo Hypersil-Hypurity C18反相柱(150mm×2.1mm内径,5μm)分离样品。采用含10mM醋酸铵(pH 3.6)-甲醇-乙腈(27:68:5,v/v/v)的流动相,以0.22ml/min的流速等度洗脱。马来酸氯丙嗪和内标的平均萃取回收率分别为81.8±2.2%和79.5±3.7%。通过电喷雾离子源在正离子选择性离子监测模式下测定马来酸氯丙嗪和内标物。该方法显示出良好的线性,范围为0.20至6.40ng/ml,r² = 0.9989。血浆中马来酸氯丙嗪的定量限为0.20ng/ml。所建立的方法已成功应用于18名健康中国男性志愿者的两种马来酸氯丙嗪制剂的生物等效性研究。