引用本文: | 任秀华,杜光,杨惠,刘东.HPLC-MS同时测定人血浆中卡马西平和苯妥英钠的血药浓度[J].中国现代应用药学,2013,30(12):1337-1342. |
| REN Xiuhua,DU Guang,YANG Hui,LIU Dong.Simultaneous Determination of Carbamazepine and Phenytoin in Human Plasma by HPLC-MS[J].Chin J Mod Appl Pharm(中国现代应用药学),2013,30(12):1337-1342. |
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摘要: |
目的 建立一种快速、灵敏并同时测定人血浆中卡马西平(CBZ)和苯妥英钠(PT)浓度的高效液相色谱-质谱联用检测方法。方法 以兰索拉唑为内标,血浆样品经乙腈沉淀后,经HPLC-MS分离分析。采用Diamonsil C18柱(2.1 mm×150 mm,5 μm),流动相:甲醇-水(含0.1%甲酸)=0.20∶0.10;流速:0.3 mL·min-1,采用电喷雾离子源(ESI),以多反应监测方式(MRM)进行正离子监测,CBZ、PT和兰索拉唑的定量分析离子对分别为m/z 237.0/194.0,253.2/182.0,392.0/188.2。结果 CBZ在40.30~20 150.00 ng·mL-1(r=0.993 7)内线性良好,为40.3 ng·mL-1,低(66.08 ng·mL-1)、中(660.8 ng·mL-1)、高(16 120 ng·mL-1)3个浓度的平均回收率RSD均<15%。PT在80.1~40 050.0 ng·mL-1(r=0.997 6)内线性良好,最低定量限为80.1 ng·mL-1,低(133.5 ng·mL-1)、中(1 335.00 ng·mL-1)、高(32 040.00 ng·mL-1)3个浓度的平均回收率RSD均<15%。结论 该方法快速简便,灵敏准确,可用于CBZ和PT同时应用时两者的血药浓度监测及其药动学研究。 |
关键词: 卡马西平 苯妥英钠 高效液相色谱串联质谱法 血药浓度监测 |
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Simultaneous Determination of Carbamazepine and Phenytoin in Human Plasma by HPLC-MS |
REN Xiuhua, DU Guang, YANG Hui, LIU Dong
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Department of Pharmacy, Tongji Hospital, Tongji Medical College of Huazhong University of Science and Technology, Wuhan 430030, China
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Abstract: |
OBJECTIVE To establish a rapid and sensitive HPLC-MS method for simultaneous quantitative determination of carbamazepine(CBZ) and phenytoin(PT) in human plasma. METHODS Plasma samples were precipitated with acetonitrile and determined by HPLC-MS using lansoprazole as an internal standard. The separation was carried out on a Diamonsil C18 column(2.1 mm×150 mm, 5 μm) with a mobile phase of methanol-water(including 0.1% formic acid)(0.20∶0.10) and with a flow rate of 0.3 mL·min-1. ESI was performed in the MRM positive mode using target ions at m/z 237.0/194.0(CBZ), 253.2/182.0(PT), and 392.0/188.2(lansoprazole), respectively. RESULTS The RSD of average recovery rate for CBZ on three levels of concentration of low(66.08 ng·mL-1), medium (660.8 ng·mL-1) and high (16 120 ng·mL-1), were <15%. The calibration curves of CBZ was obtained in the range of 40.3-20 150.0 ng·mL-1(r=0.993 7) with good linearity. The low limit of quantitation was 40.3 ng·mL-1. Meanwhile, the RSD of average recovery rate for CBZ on three levels of concentration of low (133.5 ng·mL-1), medium (1 335.00 ng·mL-1) and high (32 040.00 ng·mL-1), were also <15%. The calibration curves for PT was obtained in the range of 80.1-40 050.0 ng·mL-1(r=0.997 6) with good linearity. The low limit of quantitation was 80.1 ng·mL-1. CONCLUSION The method provides a sensitive, accurate, precise and reliable analytical procedure for the therapeutic drug monitoring of CBZ and PT simultaneously in clinic and phamacokinetic studies. |
Key words: carbamazepine phenytoin HPLC-MS therapeutic drug monitoring |