摘要
建立了离心式微固相萃取与液相色谱-质谱(LC-MS)联用,同步测定尿样和血样中5种新型合成大麻素的分析方法。尿样和血样稀释后在离心条件下通过C18离心式固相萃取柱,甲醇洗脱后LC-MS检测。结果显示,尿液基质中,5种合成大麻素在0.1~10μg/L浓度范围内线性关系良好,相关系数(R^(2))大于0.994,检出限(LODs)为0.01~0.02μg/L,定量限(LOQs)为0.05~0.08μg/L。全血基质中,5种合成大麻素在0.5~10μg/L浓度范围内线性关系良好,R^(2)大于0.992,LODs为0.05~0.15μg/L,LOQs为0.18~0.50μg/L。在尿样和全血中分别添加0.5,2,10μg/L 3个浓度水平的合成大麻素,回收率分别为81.9%~108.3%和75.0%~95.5%,相对标准偏差(RSDs)低于10%。该方法可以满足生物样品中新型合成大麻素的分析需求。
A spin-column micro-solid phase extraction coupled with LC-MS method was developed for the determination of 5 new synthetic cannabinoids in urine and blood samples.The urine or blood sample was diluted with ultrapure water and then extracted by the C18 spin column.The analytes on spin column were eluted with methanol,and then the eluate was determined by LC-MS method.For the urine matrix,the linear range of each synthetic cannabinoid was 0.1-10μg/L,with the correlation coefficients(R^(2))higher than 0.994.The limits of detection(LODs)and limits of quantification(LOQs)were 0.01-0.02μg/L and 0.05-0.08μg/L,respectively.For the blood matrix,the linear range of each synthetic cannabinoid was 0.5-10μg/L,with R^(2) higher than 0.992.LODs were 0.05-0.15μg/L and LOQs were 0.18-0.50μg/L,respectively.The recoveries of 5 analytes in the spiked urine and blood samples at three spiked levels of 0.5,2 and 10μg/L were 81.9%-108.3% and 75.0%-95.5%,respectively,with the relative standards(RSDs)less than 10%.This method is suitable for the analysis of new synthetic cannabinoids in biological samples.
作者
姚伟宣
陈楠旭
张素玲
王继业
吴元钊
王斌杰
YAO Weixuan;CHEN Nanxu;ZHANG Suling;WANG Jiye;WU Yuanzhao;WANG Binjie(Key Laboratory of Drug Prevention and Control Technology of Zhejiang Province,Zhejiang Police College,Hangzhou 310053,China;College of Malerials and Environmental Engineering,Hangzhou Dianzi University,Hangzhou 310018,China)
出处
《分析试验室》
EI
CAS
CSCD
北大核心
2023年第9期1215-1220,共6页
Chinese Journal of Analysis Laboratory
基金
浙江省重点研发计划项目(2021C03135)
浙江省基础公益研究计划分析测试项目(LGC21B050003)资助。
关键词
离心式萃取
固相萃取
合成大麻素
尿样
血样
spin column extraction
solid-phase extraction
synthetic cannabinoids
urine
blood sample
