QuEChERS结合UPLC-M S/M S检测血液中苯丙胺类及其相关9种物质

对QuEChERS前处理方法从提取、分离、净化等方面进行优化以减弱样本中的基质效应,提高灵敏度;使用提取试剂(含0.1%甲酸的乙腈:甲醇=70:30,V/V)进行提取,加入无水硫酸镁、硼酸钠、研磨珠进行提取分离,使用混合净化剂(十八烷基硅烷(C18):乙二胺-N-丙基硅烷(PSA)=1:2,m/m)进行净化,UPLC-MS/MS测定,外标法定量。结果表明:在优化条件下,苯丙胺类及其相关9种物质的色谱峰分离良好,且各标准化合物的线性相关系数均大于0.991,检出限(LODs)为0.3~1.0 ng/mL,定量限(LOQs)均为2.5 ng/mL;血液添加标准品样本在低(20 ng/mL)、中(100 ng/mL)、高(400 ng/mL)3个浓度的加标回收率为80.1%~103.1%,精密度相对标准偏差(RSD)为1.5%~8.6%;临床4份检测样本中有3份检出苯丙胺类阳性,准确率为71.5%~99.1%。所建立的QuEChERS方法与UPLC-MS/MS结合的分析方法可应用于血液样本中苯丙胺类及其相关9种药物的同时检测分析。

Analysis of nine kinds of amphetamine-type compounds in blood by method of QuEChERS combined with UPLC-MS/MS

The QuEChERS pretreatment method was optimized on extraction,separation and purification to reduce the matrix effect and improve the sensitivity.Acetonitrile containing 0.1%formic acid:methanol=70:30(V/V)was used as extraction reagent,and anhydrous magnesium sulfate,sodium borate,grinding beads were added to extract and separate.A combination of agent(octadecylsilane(C18):primary secondary amine(PSA)sorbent=1:2,m/m)was employed for cleanup.The external standard method was used for quantitative analysis combined with UPLC-MS/MS instrumental analysis.The results demonstrated that the chromatographic peaks of the amphetamine-type compounds were well separated,and the correlation coefficients of all the compounds were greater than 0.991.The limits of detection(LODs)were 0.3-1.0 ng/m L and limits of quantitation(LOQs)were 2.5 ng/m L.In addition,the recoveries of the analytes spiked into whole blood of low(20 ng/m L),medium(100 ng/m L)and high concentrations(400 ng/m L)ranged between 80.1%and 103.1%,and the relative standard deviations(RSDs)were 1.5%-8.6%.Three of the four clinical samples were positive for amphetamine and methamphetamine,with an accuracy of 71.5%-99.1%.The established QuEChERS method combined with UPLC-MS/MS can be applied to simultaneous determination of amphetamine-type compounds and nine related drugs in blood samples.