在线固相萃取-液相色谱-串联质谱法测定血液和尿液中31种有毒植物化学组分的含量  

Determination of 31 Chemical Constituents of Poisonous Plants in Samples of Blood and Urine by LC-MS/MS with Separation by Online Solid Phase Extraction

作　　者：莫静[1] 黄克建[2] 罗轩[1] 杨宁[2] 刘晓峰 李璐[2] 乔文涛[2] 朱定姬[3] MO Jing;HUANG Kejian;LUO Xuan;YANG Ning;LIU Xiaofeng;LI Lu;QIAO Wentao;ZHU Dingji(School of Chemistry and Chemical Engineering,Guangxi University,Nanning 530004,China;Evidence Identification Center,Public Security Department of Guangxi Zhuang Autonomous Region,Nanning 530012,China;Institute for the Prevention and Treatment of Occupational Diseases of Guangxi Zhuang Autonomous Region,Nanning 530021,China)

机构地区：[1]广西大学化学化工学院,南宁530004 [2]广西壮族自治区公安厅物证鉴定中心,南宁530012 [3]广西壮族自治区职业病防治研究院,南宁530021

出　　处：《理化检验（化学分册）》2019年第1期17-25,共9页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：取血液或尿液样品0.20mL,加入乙腈0.60mL,涡旋振荡1min,并离心10min,取上清液0.40mL,加入10mol·L^(-1)乙酸铵溶液(pH 7.0)1.1mL,振荡1min,用0.22μm滤膜过滤后,溶液经HLB在线固相萃取柱富集纯化,所用流动相A为水,B为甲醇,C为乙腈。所得淋出液经Poroshell 120EC-C18色谱柱并用流动相A 10mol·L^(-1)乙酸铵溶液和流动相B乙腈(上述二流动相中均含φ0.1%甲酸)进行梯度洗脱,使所测定的31种有毒植物的化学组分达到分离,并进行质谱测定。所测定的31种目标物的质量浓度在一定范围内与其峰面积之间呈线性关系,其检出限(3S/N)在0.01～5.00μg·L^(-1)之间。分别以上述两种样品为基体,用标准加入法进行回收试验,测得31种化合物在血液样品中的回收率在90.4%～107%之间,在尿液样品中的回收率在90.0%～103%之间。测定值的相对标准偏差(n=6)依次在0.2%～2.6%,0.3%～2.9%之间。0.20 mL of the sample of blood or urine was taken and shaked vortically for 1 min with 0.60 mL of acetonitrile,and then centrifuged for 10 min.A portion(0.40 mL)of the supernatant was taken and diluted with1.1 mL of 10 mol·L^-1 CH3COONH4 solution(pH 7.0);after shaking for 1 min,the solution was filtered through0.22μm filtering membrane and the filtrate was passed through the HLB online solid phase extraction column for enriching and purifying the 31 analytes(i.e.,the constituents of poisonous plants)by elution with mobile phases of(A)water,(B)methanol and(C)acetonitrile.The eluates obtained were then separated by gradient elution using Poroshell 120 EC-C18 column as stationary phase and(A)10 mol·L^-1 CH3COONH4 solution,(B)acetonitrile as mobile phases,both of which contained 0.1%(φ)of formic acid.The 31 analytes in the eluates were then determined by tandem MS.Linear relationships were obtained between values of peak areas of the 31 analytes and their mass concentrations in definite ranges,with detection limits(3 S/N)in the range of 0.01-5.00μg·L^-1.Test for recovery was made by standard addition on the base of blood sample or urine sample as matrixes separately,giving results of recovery of the 31 compounds in the range of 90.4%-107% for blood sample and of 90.0%-103%for urine sample.Values of RSDs(n=6)ranged from 0.2% to 2.6% and from 0.3% to 2.9% for the 2 kinds of samples respectively.

关 键 词：在线固相萃取 液相色谱-串联质谱法 化学组分 有毒植物 血液 尿液 

分 类 号：O657.63[理学—分析化学]