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作 者:李力[1] 肖昌钱[1] 朱逢佳[1] 廉洪[1] 韩奇[1] 刘炜[1]
机构地区:[1]浙江医院药剂科,杭州310013
出 处:《中国现代应用药学》2014年第12期1496-1499,共4页Chinese Journal of Modern Applied Pharmacy
基 金:"重大新药创制"科技重大专项(2013ZX09303005);国家自然科学基金(31201040)
摘 要:目的 建立LC-MS/MS方法测定人血浆中阿罗洛尔的浓度。方法 人血浆样品用乙酸乙酯提取后,选用ZORBAX Extend C18(2.1 mm×100 mm,3.5-m)色谱柱,以乙腈-水(80∶20,含0.1%甲酸)为流动相,流速为0.30 m L·min^-1,采用电喷雾离子化源,正离子方式,多反应监测(MRM)扫描方式进行监测,用于定量分析的离子反应分别为m/z372.3→315.9(阿罗洛尔)和m/z 267.2→145.0(内标阿替洛尔)。结果 血浆中阿罗洛尔的线性范围为0.5~1 000 ng·m L^-1(r=0.995 2),定量下限为0.5 ng·m L^-1;日内、日间RSD均〈15%;低、中、高3个浓度的提取回收率分别为(80.6±1.6)%,(83.2±3.1)%和(87.5±4.5)%。结论 该方法快速、灵敏、准确,专属性强,重复性好,适用于人血浆中阿罗洛尔浓度的测定,可应用于阿罗洛尔的血药浓度检测和药动学研究。OBJECTIVE To develop a LC-MS/MS method for determination of arotinolol concentration in human-plasma. METHODS The plasma samples were processed with ethyl acetate extraction and separated on ZORBAX Extend C18 column(2.1 mm×100 mm, 3.5 μm) and eluted with acetonitrile-water(80∶20, containing 0.1% formic acid). Detection of the analyte was achieved using positive ion electrospray ionization(ESI) in the multiple reaction monitoring(MRM) mode. The MS/MS ion transitions monitored were m/z 372.3→m/z 315.9 and m/z 267.2→m/z 145.0 for arotinolol and internal standard, respectively. RESULTS The linear calibration curve of arotinolol was obtained concentration range of 0.5-1 000 ng·m L^-1(r=0.995 2), with the lower limit of quantitation of 0.5 ng·m L^-1. Intra-day and inter-day relative standard deviations were both 15%. The recoveries of low, middle and high concentrations were(80.6±1.6)%,(83.2±3.1)% and(87.5±4.5)%, respectively. CONCLUSION The established method is rapid, sensitive, accurate, specific and reliable, and suitable for the determination of arotinolol in human plasma and pharmacokinetic study.
分 类 号:R917.101[医药卫生—药物分析学]
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