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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 |
| 阅读数： | 404 次 |
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