高效液相色谱-大气压化学电离源-质谱法测定人血浆中帕洛诺司琼浓度
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江苏省卫生厅医学科技发展基金资助(P20080)


Determination of palonosetron in plasma by HPLC-APCI-MS
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    摘要:

    目的:建立液质联用法(HPLC-MS/MS)测定人血浆中帕洛诺司琼浓度的方法-方法:色谱条件为Hypersil GOLD(150.0 mm × 4.6 mm,5 μm)柱,流动相为0.2%醋酸铵水溶液(含0.1%甲酸)-甲醇(50∶50),质谱条件为大气压化学电离源(APCI源),血浆样品中加入内标,碱化后用乙酸乙酯提取,浓缩后采用高效液相色谱-质谱联用进行测定-结果:血浆样品中帕洛诺司琼浓度在0.04~20.00 ng/ml的线性范围内关系良好(r = 0.999 9),定量下限为0.04 ng/ml;低-中-高浓度的回收率-批内及批间精密度均符合生物样本测定方法学要求-结论:本方法灵敏度高-专属性强-重现性好,可用于帕洛诺司琼药代动力学研究及血药浓度监测-

    Abstract:

    Objective:To establish a determination method of palonosetron level in plasma. Methods:LC conditions were as follows: Hypersil GOLD(150 mm × 4.6 mm, 5 μm)was used with the mobile phase consisting of acetateamine buffer (0.1% formic acid )-method(50∶50). Equipped with an atmospheric pressure chemical ionization(APCI) source was used as detector. The plasma samples added with internal standard were extracted with Acetic Ether, then concentrated and determined by LC-MS/MS. Results:The linear range of palonosetron was 0.04~20.00 ng/ml . The lower limit of quantification(LLOQ) was 0.04 ng/ml. The recoveries of palonosetron at low, middle and high concentration and the intra-day and inter-day RSDs all met the standards. Conclusion:The established method is sensitive, specific, reproducible and suitable for studies of pharmacokinetics and detection of plasma drug concentration of palonosetron.

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吴德芹,陈安九,张宏文,葛 萍,王永庆,欧 宁,孟 玲.高效液相色谱-大气压化学电离源-质谱法测定人血浆中帕洛诺司琼浓度[J].南京医科大学学报(自然科学版),2011,(6):903-906

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  • 收稿日期:2010-12-29
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