Development and in-house validation of a sensitive LC-MS/MS method for simultaneous quantification of gelsemine, koumine and humantenmine in porcine plasma

被引：18

作者：

Yang, Kun ^{[1
]}

Long, Xue-Ming ^{[2
]}

Liu, Yan-Chun ^{[1
]}

Chen, Fu-Hua ^{[2
]}

Liu, Xiao-Feng ^{[1
]}

Sun, Zhi-Liang ^{[1
,3
]}

Liu, Zhao-Ying ^{[1
,3
,4
]}

机构：

[1] Hunan Agr Univ, Coll Vet Med, Hunan Engn Res Ctr Vet Drug, Changsha 410128, Hunan, Peoples R China

[2] Inst Hunan Prov Vet Drugs & Feed Supervis, Changsha 410006, Hunan, Peoples R China

[3] Hunan Agr Univ, Coll Vet Med, Hunan Coinnovat Ctr Utilizat Bot Funct Ingredient, Changsha 410128, Hunan, Peoples R China

[4] Hunan Agr Univ, Natl & Local Union Engn Res Ctr Vet Herbal Med Re, Changsha 410128, Hunan, Peoples R China

来源：

JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES | 2018年 / 1076卷

基金：

国家重点研发计划;

关键词：

Indole alkaloid; Gelsemine; Gelsemium elegans; Plasma; Koumine; Humantenmine; TANDEM MASS-SPECTROMETRY; TIME-OF-FLIGHT; RAT PLASMA; CHROMATOGRAPHY; ALKALOIDS; QUADRUPOLE; COMPONENTS; ELEGANS;

D O I：

10.1016/j.jchromb.2018.01.019

中图分类号：

Q5 [生物化学];

学科分类号：

071010 ; 081704 ;

摘要：

Three monomers of G. elegans indole alkaloids (gelsemine, koumine and humantenmine) were simultaneously detected in porcine plasma for the first time with the development and validation of a sensitive and reliable LC-ESI-MS/MS method. Using a gradient mobile phase at a constant flow rate of 0.2 mL/min via electrospray ionization (positive ion mode) in a multiple reaction monitoring (MRM) scan, gelsemine, koumine and humantenmine were eluted, separated and detected at an appropriate retention time. The porcine plasma was prepared using protein precipitation with 1% formic acid-acetonitrile: methanol (2:1, v/v). Using matrix-matched calibration curves and weighted least squares linear regression, a good linearity (r(2) > 0.99) was achieved with a concentration range of 0.1-200 mu g/L for gelsemine, koumine and humantenmine; estimated LOD and LOQ values were 0.10 mu g/L and 0.2 mu g/L, respectively. The mean of the recoveries was in the range of 82.68-400.35% of porcine plasma at four different levels, and the intra-day and inter-day precision (CV) were lower than 15% with a range of 2.46-8.76% and 2.73-10.83%, respectively. The proposed method has proved to be suitable for accurate, quantitative determination of gelsemine, koumine and humantenmine in porcine plasma.

引用

页码：54 / 60

页数：7