LC-MS/MS法测定人血浆中利培酮及9-羟基利培酮的浓度
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篇名: LC-MS/MS法测定人血浆中利培酮及9-羟基利培酮的浓度
TITLE:
摘要: 目的:建立同时测定人血浆中利培酮及9-羟基利培酮浓度的方法。方法:血浆样品经液-液萃取后,以AF2672为内标,采用液相色谱-串联质谱(LC-MS/MS)法测定。色谱柱为XtimateTM C18,流动相为乙腈-10 mmol/L乙酸铵溶液(含0.1%甲酸)(37 ∶ 63,V/V,pH=3.2),流速为0.25 mL/min,柱温为40 ℃,进样量为6 μL。采用电喷雾电离源,以多反应离子监测进行正离子扫描,用于定量分析的离子对分别为m/z 411.26→191.02(利培酮)、m/z 427.21→206.91(9-羟基利培酮)、m/z 418.00→175.95(内标)。结果:利培酮、9-羟基利培酮血药浓度分别在0.2~50.0、1.0~200.0 ng/mL范围内线性关系良好(r分别为0.999 7、0.998 7);日内、日间RSD<15%,方法回收率分别为92.42%~104.81%、94.51%~100.57%,基质效应分别为98.33%~107.09%、91.05%~105.80%,提取回收率分别为78.11%~92.62%、76.32%~85.09%。采用该法测得78例精神分裂症患者体内利培酮和9-羟基利培酮的血药浓度分别为(13.58±8.31)、(25.62±15.52)ng/mL。结论:该方法操作简便、专属性强、灵敏度高,可用于口服利培酮患者的常规治疗药物监测和急性中毒分析。
ABSTRACT: OBJECTIVE: To establish the method for simultaneous determination of risperidone (RIS) and 9-hydroxyrisperidone (9-OH-RIS) in human plasma. METHODS: After liquid-liquid extraction of plasma sample, using AF2672 as internal standard (IS), LC-MS/MS was adopted. The determination was performed on XtimateTM C18 column with mobile phase consisted of acetonitrile-10 mmol/L ammonium acetate solution (containing 0.1% formic acid)(37 ∶ 63,V/V,pH=3.2) at the flow rate of 0.25 mL/min. The column temperature was 40 ℃, and the sample size was 6 μL. The ESI was equipped and quantitative analysis was operated in positive ion and MRM mode. The mass transition ion-pairs were followed as m/z 411.26→191.02 for RIS, m/z 427.21→206.91 for 9-OH-RIS and m/z 418.00→175.95 for IS. RESULTS: The linear range of RIS was 0.2-50.0 ng/mL (r=0.999 7) and 9-OH-RIS was 1.0-200.0 ng/mL (r=0.998 7). RSDs of inter-day and intra-day were all lower than 15%, and the method recoveries were 92.42%-104.81% and 94.51%-100.57%; matrix effects were 98.33%-107.09% and 91.05%-105.80%; extraction recoveries were 78.11%-92.62% and 76.32%-85.09%, respectively. The plasma concentrations of RIS and 9-OH-RIS in 78 schizophrenic patients were (13.58±8.31) and (25.62±15.52) ng/mL. CONCLUSIONS: The developed method is simple, sensitive and specific, which is suitable for routine drug monitoring and acute toxic analysis in patients receiving risperidone.
期刊: 2017年第28卷第26期
作者: 楼江,严伟,王刚,王飞,王峰,李焕德
AUTHORS: LOU Jiang,YAN Wei,WANG Gang,WANG Fei,WANG Feng,LI Huande
关键字: 液相色谱-串联质谱法;利培酮;9-羟基利培酮;血药浓度
KEYWORDS: LC-MS/MS; Risperidone; 9-hydroxyrisperidone; Plasma concentration
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