高效液相色谱-串联质谱法测定豚鼠血浆中的合成辣椒素  

Determination of nonivamide in guinea pig plasma by high performance liquid chromatography-tandem mass spectrometry

作　　者：张倩 李海芸 张泗达 陈东 徐建富 张瑞华 ZHANG Qian;LI Haiyun;ZHANG Sida;CHEN Dong;XU Jianfu;ZHANG Ruihua(State Key Laboratory of NBC Protection for Civilian,Beijing 102205,China)

机构地区：[1]国民核生化灾害防护国家重点实验室,北京102205

出　　处：《分析试验室》2025年第1期83-88,共6页Chinese Journal of Analysis Laboratory

基　　金：国民核生化灾害防护国家重点实验室基金(SKLNBC2021-11)资助。

摘　　要：建立了高效液相色谱-串联质谱(HPLC-MS/MS)测定豚鼠血浆中痕量合成辣椒素(NOV)的方法。以天然辣椒素(CAP)为内标,血浆样品经乙腈沉淀蛋白、高速离心、真空干燥浓缩、流动相复溶,制备待检样品。采用Agilent EclipsePlus C18色谱柱(2.1 mm×150 mm,1.8μm),以0.1%甲酸水溶液和乙腈为流动相,在电喷雾离子源(ESI)、多反应监测(MRM)模式下检测。采用梯度洗脱程序,待测物NOV及内标物CAP出峰时间均在5.31 min。选择m/z 294.2→137.1作为NOV定量离子,m/z 306.2→137.1为内标物定量离子。NOV在豚鼠血浆中的基质效应为98.6%~104.0%,回收率为110.4%~117.4%,日间相对标准偏差为0.2%~2.6%。在0.05~50 ng/mL浓度范围内线性关系良好,相关系数(R2)为0.9998,定量限为0.05 ng/mL。该方法能够满足血浆中痕量NOV的检测需求,适用于开展新型控暴剂NOV吸入暴露后的定量分析和相关机制研究。A method was established for the determination of trace nonivamide(NOV)in guinea pig plasma by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Capsaicin(CAP)was chosen as the internal standard.Protein was precipitated with acetonitrile in the plasma samples,then the samples were centrifuged at high speed,dried and concentrated under vacuum condition,and finally prepared by mobile phase reconstitution.The Agilent EclipsePlus C18 column(2.1 mm×150 mm,1.8μm)was used.The mobile phases consisted of acetonitrile and water containing 0.1%formic acid.The electrospray ionization(ESI)source and multiple reaction monitoring(MRM)mode were used for the detection.Using gradient elution program,the peak time of both NOV and the internal standard(CAP)was 5.31 min.m/z 294.2→137.1 was selected as the quantification ion of NOV,and m/z 306.2→137.1 as the internal standard quantification ion.The matrix effects of NOV in guinea pig plasma were 98.6%-104.0%,the recoveries were 110.4%-117.4%,and the inter-day relative standard deviations were 0.2%-2.6%.The linear relationship was good in the concentration range of 0.05-50 ng/mL,with the correlation coefficient(R~2)of 0.9998.The limit of quantification was 0.05 ng/mL.This method can meet the detection needs of trace NOV in plasma and can be used to carry out the quantitative analysis and related mechanism research of NOV after inhalation exposure as a novel riot control agent.

关 键 词：高效液相色谱-串联质谱(HPLC-MS/MS) 豚鼠血浆 合成辣椒素(NOV) 天然辣椒素(CAP) 

分 类 号：O657.63[理学—分析化学]