血液中磺酰脲类除草剂液相提取HPLC/MS检测  

Simultaneous Determination of Sulfonylurea Herbicides in Human Blood by High Performance Liquid Chromatography-mass Spectrometry

作　　者：杨士云[1] 王燕燕[2] 乔静[1] 

机构地区：[1]北京市公安局法医中心,北京100192 [2]北京市公安局东城分局,北京100007

出　　处：《现代科学仪器》2013年第2期148-152,共5页Modern Scientific Instruments

摘　　要：以添加甲磺隆、苯磺隆、氯磺隆、玉嘧磺隆标准液的人体血液为样本,建立了血液样本中此4种磺酰脲类除草剂的液相提取-高效液相色谱/质谱(HPLC/MS)定性、定量分析方法。在对萃取溶剂、pH环境等条件进行考查后,以2×8mL乙酸乙酯为提取溶剂,超声震荡提取10min、离心,取上层有机相挥干、乙腈定容后进行LC/MS-MRM分析,采用该方法对血液添加样本在10～1000ng/mL范围内做标准曲线,相关系数在0.999到0.9998之间,相对标准偏差均在13%以内,准确性在88%～110%之间,回收率均在63%～83%之间,方法最低定量限为10ng/mL,最低检测限为2～5ng/mL。该方法稳定,简单,灵敏度高,可用于对人体血液中磺酰脲类除草剂的检测和分析。An high performance liquid chromatography-mass spectrometry（HPLC-MS） method was developed for the confirmation and quantitation of 4 sulfonylurea herbicides including Tribenuron,Metsulfuron methyl,Thifensulfuron and Rimsulfuron in human blood.Some extraction parameters such as extraction solvent,pH value were investigated.The samples were extracted with ethyl acetate,ultrasonic for about 10 minutes,dried the upper organic phase after centrifuge,dissolved by acetonitrile,separated with HPLC and detected with MS in multiple reaction monitoring（MRM）mode via positive electrospray ionization（ESI＋）.The method was used for spiked blood analysis,the standard calibration curves for 4 sulfonylurea herbicides all showed linear over the range of 10-1000ng/mL with the correlation coefficients between0.999and0.9998.The relative standard deviation（RSD） was under 13%,the accuracies varied from 88% to 110%,the recoveries were in the range of 63%-83%,the limit of detection（LOD） was 2-5ng/mL.The results indicated that this method is easier,more sensitive,can be applied to detecting trace amount of Sulfonylurea herbicides in human blood.

关 键 词：血液 磺酰脲类类除草剂 LC MS 

分 类 号：O657.63[理学—分析化学] D919.1[理学—化学]