UPLC-MS/MS法测定人血浆中奥氮平、利培酮和帕潘立酮的浓度
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篇名: UPLC-MS/MS法测定人血浆中奥氮平、利培酮和帕潘立酮的浓度
TITLE:
摘要: 目的:建立同时测定人血浆中奥氮平、利培酮和帕潘立酮浓度的方法。方法:血浆样品经液-液萃取后,以盐酸丁螺环酮为内标,采用超高效液相色谱-串联质谱法测定。色谱柱为ACQUITY UPLCTM BEH C18,流动相为甲醇-0.01 mol/L甲酸铵水溶液,梯度洗脱,流速为0.2 mL/min,柱温为45 ℃,进样量为5 μL。采用电喷雾离子源,以多反应监测模式进行正离子扫描,用于定量分析的离子对分别为m/z 313.29→256.25(奥氮平)、m/z 411.42→191.19(利培酮)、m/z 427.45→207.18(帕潘立酮)和m/z 386.43→122.37(内标)。结果:奥氮平、利培酮、帕潘立酮血药浓度分别在0.426~108.954、0.213~54.476、0.213~54.476 ng/mL范围内线性关系良好;日内、日间RSD<20%,方法回收率分别为83.3%~112.9%,90.0%~109.8%和95.2%~114.9%,提取回收率分别为65.5%~95.0%、73.9%~98.5%和73.6%~99.4%,基质效应和稀释效应均不影响待测物血药浓度的测定。采用该法测得100例精神分裂症患者奥氮平、利培酮和帕潘立酮的血药浓度分别为(103.3±73.6)、(13.1±13.1)和(23.2±20.0)ng/mL。结论:该方法简单、快速、灵敏、特异性高,可用于奥氮平、利培酮和帕潘立酮血药浓度测定及药动学研究。
ABSTRACT: OBJECTIVE: To develop a method for the concentration determination of olanzapine, risperidone and paliperidone in human plasma. METHODS: After liquid-liquid extraction, using buspirone hydrochloride as internal standard, the concentration of plasma sample was determined by UPLC-MS/MS. The determination was performed on ACQUITY UPLCTM BEH C18 column with mobile phase consisted of methanol-0.01 mol/L ammonium formate solution (gradient elution) at flow rate of 0.2 mL/min. The column temperature was 45 ℃, and sample size was 5 μL. The electrospray ionization source was adopted for positive ion scanning under MRM mode. Ion-pairs for quantitative analysis were as follows: m/z 313.29→256.25 (olanzapine), m/z 411.42→191.19 (risperidone), m/z 427.45→207.18 (paliperidone) and m/z 386.43→122.37 (internal standard). RESULTS: The linear ranges of olanzapine, risperidone and paliperidone were 0.426-108.954, 0.213-54.476, 0.213-54.476 ng/mL, respectively. RSDs of inter-day and intra-day were all lower than 20%. The recoveries of them ranged 83.3%-112.9%, 90.0%-109.8% and 95.2%-114.9%, respectively. Extraction recoveries ranged 65.5%-95.0%, 73.9%-98.5% and 73.6%-99.4%, respectively. Both plasma matrix effect and dilute effect didn’t influence the determination of plasma concentration. The plasma concentrations of olanzapine, risperidone and paliperidone in 100 schizophrenia patients were (103.3±73.6),(13.1±13.1)and(23.2±20.0)ng/mL, respectively. CONCLUSIONS: The method is simple, rapid, sensitive and specific. It can be used for the determination of plasma concentration and pharmacodynamic study of olanzapine, risperidone and paliperidone.
期刊: 2017年第28卷第8期
作者: 丰丽莼,杨博涵,王雪芹,郭强
AUTHORS: FENG Lichun,YANG Bohan,WANG Xueqin,GUO Qiang
关键字: 奥氮平;利培酮;帕潘立酮;超高效液相色谱-串联质谱法;血药浓度
KEYWORDS: Olanzapine; Risperidone; Paliperidone; UPLC-MS/MS; Plasma concentration
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