Sichuan da xue xue bao. Yi xue ban = Journal of Sichuan University. Medical science edition · 2012
[Determination of probucol in human plasma by HPLC-MS/MS].
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Xie Kun, Xiang Jin, Yu Qin, Liang Mao-Zhi, Nan Feng, Qin Yong-Ping
Аннотация
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 x 4.6 mm, 5 microm) 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.
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 x 4.6 mm, 5 microm) 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.