HPLC-MS/MS测定大鼠脑脊液中4-(4-氨基苯基)丁酸浓度  

Determination of 4-(4-Aminophenyl) Butyric Acid in Rats’ Cerebrospinal Fluid by HPLC-MS/MS

作　　者：邱政辉 赵萌 孔珊珊 范兰兰 吴鑫慧 叶晓霞 QIU Zhenghui;ZHAO Meng;KONG Shanshan;FAN Lanlan;WU Xinhui;YE Xiaoxia(School of Pharmaceutical Sciences,Wenzhou Medical University,Wenzhou,China 325035;Lianyungang Maternal and Child Health Hospital,Lianyungang,China 222000)

机构地区：[1]温州医科大学药学院,浙江温州325035 [2]连云港市妇幼保健院,江苏连云港222000

出　　处：《温州大学学报（自然科学版）》2022年第2期38-43,共6页Journal of Wenzhou University(Natural Science Edition)

基　　金：浙江省自然科学基金(LY17B020009);温州市科技局公益社会发展项目(Y20160084);浙江省医药卫生科技计划项目(2019KY097)。

摘　　要：给出一种HPLC-MS/MS法测定大鼠脑脊液中4-(4-氨基苯基)丁酸浓度的分析方法.采用Waters Atlantis;-C;色谱柱,大鼠脑脊液样品经乙腈沉淀蛋白后进样分析,以含0.1%甲酸的水-乙腈为流动相进行梯度洗脱,流速为0.4 m L/min,柱温为25℃;采用离子肼离子源、多离子反应监测、正离子扫描进行测定.结果显示,4-(4-氨基苯基)丁酸浓度在30―10 000 ng/mL内线性关系良好,标准曲线为y=218 080x+27 920(R;=0.999 0),定量下限为30 ng/mL;在低、中和高浓度下,4-(4-氨基苯基)丁酸的提取回收率在79.26%―85.34%之间,日内、日间相对误差和变异系数均小于15%,且所有质控样品在考察的条件下均稳定性良好.该方法简便快捷、准确度高、灵敏度好,可满足4-(4-氨基苯基)丁酸的药物代谢动力学和药理学研究的需要.This paper established an HPLC-MS/MS method for the determination of the content of4-(4-Aminophenyl) butyric acid in rats’cerebrospinal fluid.The rats’cerebrospinal fluid was extracted by acetonitrile and separated with Waters Atlantis;-C;column.Water and acetonitrile (both containing 0.1%formic acid) were used as the mobile phase for gradient elution at the flow rate of 0.4 mL/min and the column temperature of 25℃.MS detection was carried out by using ion trap ionization source,multiple reaction monitoring (MRM) mode and positive ion scanning.The results showed that the linear relationship was good when the mass concentration of 4-(4-Aminophenyl) butyric acid was in the range of 30―10 000 ng/mL,and the calibration curve was y=218 080x+27 920 (R~2=0.999 0).The lower limit of quantitation was 30 ng/mL.At low,medium and high concentrations,the extraction recoveries were in the range of 79.26%―85.34%,and the intra-day and inter-day relative error and coefficient of variation were within 15%.4-(4-Aminophenyl)butyric acid was stable under the tested conditions at three QC levels.The HPLC-MS/MS method is simple,rapid and accurate,and it can meet the need of pharmacokinetic and pharmacological study of4-(4-Aminophenyl) butyric acid.

关 键 词：高效液相色谱-串联质谱 4-(4-氨基苯基)丁酸 脑脊液 

分 类 号：O657[理学—分析化学]