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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 |
| 阅读数： | 827 次 |
| 本月下载数： | 8 次 |
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