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	超高效液相色谱串联质谱法检验全血中三种合成大麻素
其他题名	Determination of synthetic cannabinoids in blood by UPLC/MS/MS
	林宽 1; 王继芬 1; 吕昱帆 1; 徐多麒 1; 张蕾萍 2
来源期刊	分析试验室
ISSN	1000-0720
出版年	2017
卷号	36 期号:8 页码:894-899
中文摘要	建立了同时测定全血中合成大麻素JWH-018,JWH-250和AM-2201超高效液相色谱-三重四极杆质谱(UPLC-TQ/MS)快速检验方法。分别考察了沉淀蛋白法,改良后的QuEChERS方法和Oasis HLB固相萃取3种前处理方法,以回收率为考察标准,比较了3种前处理方法的优缺点。沉淀蛋白法使用乙腈沉淀血液中的蛋白质,振荡、离心、过膜后直接进样;改良后的QuEChERS方法采用无水MgSO_4平衡水相;固相萃取选用HLB柱,对pH、淋洗液、缓冲液等条件进行优化,选用pH 9的硼砂-硼酸(4:1, V/V)缓冲液,甲醇-水(5:95, V/V)溶液为淋洗液,0.1%甲酸-乙腈(1:4, V/V)为洗脱液。选用ZORBAX Eclipse Plus C_(18)色谱柱,以A相0.1%甲酸水和B相0.1%甲酸-乙腈作为流动相,进行梯度洗脱。采用液相色谱-串联质谱仪的电喷雾电离,正离子模式扫描,多反应监测(MRM)模式检测合成大麻素JWH-018,JWH-250及AM-2201。结果表明,3种合成大麻素在其各自的浓度范围内线性关系良好(R~2>0.999);3个添加水平(5,50,100 ng/mL)下,固相萃取方法回收率在70.1% ~ 98.5%之间,改良后的QuEChERS方法回收率在80.3% ~ 108.6%之间,沉淀蛋白法回收率在62.0% ~ 92.3%之间,3种合成大麻素检出限(S/N=3)在0.01 ~ 0.05 ng/mL范围内,定量限(S/N=10)在0.05~ 0.1 ng/mL范围内。
英文摘要	Three pretreatment methods which are protein precipitation, optimized QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) and solid-phase extraction are studied comparatively. Optimized QuEChERS method for the simultaneous determination of synthetic cannabinoids, including JWH-018, JWH-250 and AM-2201 in human blood samples by ultra-performance chromatography-tandem mass spectrometry (UPLC-TQ/MS) has been established. The recovery was taken as investigated standard, to evaluate and compare the advantages and disadvantages of those three methods. The protein precipitation method: the blood samples were extracted with acetonitrile by vortex and vibrate technique, then direct injection after membrane; The optimized QuEChERS method: the blood samples were dehydrated by adding anhydrous magnesium sulfate; Using Oasis HLB cartridges for soild phase extaction (SPE); optimizing conditions of pH, eluent and buffer conditions. At last, we used the pH 9 borax-borate (4:1; V/V) buffer solution, with methanol-water(5:95, V/V)as leacheate, with 0.1% formic acid and acetonitrile (1:4, V/V) as eluent. A ZORBAX Eclipse Plus C_(18) column was used. The mobile phases consisted of water containing 0.1 % formic acid (mobile phase A) and 0.1 % formic acid-acetonitrile (mobile phase B), gradient elute. MS-MS in the multiple reaction monitoring (MRM) mode was performed in positive electrospray ionization (ESI~+). The calibration graphs were linear in their in their concentration ranges with the correlation coefficients (R~2) more than 0.999. The limits of detection (LODs) of three methods were in the range of 0.01~0.05 ng/mL (S/N=3). The average recoveries of protein precipitation method for target drugs were 62.0% to 92.3%. The average recoveries of optimized QuEChERS for target drugs were 80.3% to 108.6%. The average recoveries of SPE for target drugs were 70.1% to 98.5%, while limits of quantification (LOQ) were in the range of 0.05-0.1 ng/mL (S/N=10).
中文关键词	合成大麻素 ; 超高效液相色谱-串联质谱 ; 沉淀蛋白法 ; QuEChERS方法 ; 固相萃取
英文关键词	Synthetic cannabinoids Ultra-performance chromatography-tandem mass spectrometry Protein precipitation QuEChERS Solid-phase extraction
语种	中文
国家	中国
收录类别	CSCD
WOS类目	PHARMACOLOGY PHARMACY
WOS研究方向	Pharmacology & Pharmacy
CSCD记录号	CSCD:6042784
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/235863
作者单位	1.中国人民公安大学刑事科学技术学院, 北京 100038, 中国; 2.公安部物证鉴定中心, 北京 100038, 中国
推荐引用方式 GB/T 7714	林宽,王继芬,吕昱帆,等. 超高效液相色谱串联质谱法检验全血中三种合成大麻素[J],2017,36(8):894-899.
APA	林宽,王继芬,吕昱帆,徐多麒,&张蕾萍.(2017).超高效液相色谱串联质谱法检验全血中三种合成大麻素.分析试验室,36(8),894-899.
MLA	林宽,et al."超高效液相色谱串联质谱法检验全血中三种合成大麻素".分析试验室 36.8(2017):894-899.