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谢琨, 向瑾, 余勤, 等. HPLC-MS/MS法测定人血浆中普罗布考浓度[J]. koko体育app 学报（医学版）, 2012, 43(5): 775-778.
引用本文: 谢琨, 向瑾, 余勤, 等. HPLC-MS/MS法检测法人血浆中普罗布考盐浓度[J]. 重庆学校学报（生物学版）, 2012, 43(5): 775-778.
XIE Kun, XIANG Jin, YU Qin, et al. Determination of Probucol in Human Plasma by HPLC-MS/MS[J]. Journal of Sichuan University (Medical Sciences), 2012, 43(5): 775-778.
Citation: XIE Kun, XIANG Jin, YU Qin, et al. Determination of Probucol in Human Plasma by HPLC-MS/MS[J]. Journal of Sichuan University (Medical Sciences), 2012, 43(5): 775-778.

HPLC-MS/MS法测定人血浆中普罗布考浓度

Determination of Probucol in Human Plasma by HPLC-MS/MS

  • 摘要: 目的 建立高效液相色谱-串联质谱（HPLC-MS/MS）技术测定人血浆中普罗布考浓度的方法。 方法 血浆经乙酸乙酯：二氯甲烷（1：1，V/V）提取后，采用HPLC-MS/MS测定。以ultimate CN（50 mm×4.6 mm，5 μm）为色谱柱，乙腈：水：氨水=97：3：0.05（甲酸调pH=7.20）为流动相进行分离。质谱采用负离子模式检测，以大黄素甲醚为内标，检测离子515.5→236.1（普罗布考）和283.0→239.9（内标）。 结果 普罗布考在2.5~6000 ng/mL范围内线性关系良好，最低定量限为2.5 ng/mL，方法回收率在93.02%~104.12%之间，日内、日间精密度分别小于4.67%及5.72%。 结论 本研究所建立的方法准确、灵敏，可用于普罗布考血药浓度测定及药代动力学研究。  
    Abstract: Objective To develop a specific and sensitive method for the determination of probucol in human plasma using HPLC-MS/MS technique. Methods Probucol were extracted from plasma by ethyl ether:dichloromethane (1:1, V/V), with physcion as an internal standard. The analytes went through the column of ultimate CN (50 mm×4.6 mm, 5 μm) with mobile phase acetonitrile:water:ammonia water=97:3:0.05 (adjusted pH=7.2 with formic acid). Probucol was analyzed with a negative mode. The ion pairs being detected were 515.5→236.1 (probucol) and 283.0→239.9 physcion, respectively. Results The established method was able to determine probucol in human plasma over the range of 2.5-6000 ng/mL, with a method recovery ranging from 93.02% to 104.12%. The intra and inter day variances were below 4.67% and 5.72%. Conclusion The HPLC-MS/MS method for analyzing probucol was validated. It is sensitive and suitable for pharmacokinetic studies of probucol.  
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