干旱区生态环境知识资源中心(Arid): 超高效液相色谱-三重四极杆质谱法检测血中脱乙基扎来普隆

Arid

	超高效液相色谱-三重四极杆质谱法检测血中脱乙基扎来普隆
其他题名	Determination of desethylzaleplon in plasma by UPLC/MS/MS
	徐多麒 1; 王继芬 1; 张蕾萍 2; 林宽 1
来源期刊	分析试验室
ISSN	1000-0720
出版年	2016
卷号	35 期号:3 页码:280-282
中文摘要	建立了全血中脱乙基扎来普隆液相色谱-串联质谱检验法。对pH、淋洗液、缓冲液等条件进行优化,实验选用HLB柱,pH 9硼酸盐缓冲溶液,氨水-甲醇水为淋洗液,乙腈为洗脱液,选用ZORBAX Eclipse Plus C_(18)色谱柱,以A相0.1%甲酸和B相乙腈作为流动相,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,MRM模式检测脱乙基扎来普隆。在最优条件下,全血中脱乙基扎来普隆质量浓度在0.1~100 ng/mL范围内有良好线性关系,保留时间为1.95 min。回归方程为y=9971.2rho-1 813.8,检出限0.1 ng/mL。回收率90%以上,日内与日间精密度均小于10%。方法适用于全血中的脱乙基扎来普隆检测。
英文摘要	We established a liquid chromatography tandem mass spectrometry (UPLC/MS/MS) assay for the determination of zaleplon main metabolite desethylzaleplon in plasma samples. The target drugs were extracted from plasma and then detected with liquid chromatography tandem mass spectrometry (UPLC/MS/MS). The SPE purification was performed with Oasis HLB 3mL cartridges previously conditioned with methanol and equilibrated with buffer solution. The mixtures of sample and buffer were loaded on the cartridge and slowly passed through the bed without vacuum. Then the cartridges column was rinsed sequentially with buffer solution and ammonia in methanol-water. After drying the column, the retained drugs were eluted with acetonitrile. The mobile phases consisted of acetonitrile (mobile phase B) and water containing 0.1% formic acid (mobile phase A). MS-MS in the multiple reaction monitoring (MRM) mode was performed in positive electrospray ionization (ESI~+). The retention time of desethylzaleplon was 1.95 min. The linear relationship was excellent between 0.1~100 ng/mL. Regression equation was y=9 971.2rho-1 813.8 and the limit of detection for desethylzaleplon was 0.1 ng/mL. The recovery of desethylzaleplon was more than 90%. The inter-day and intra-day precisions were less than 10%. This rapid, accurate and sensitive method can be used in forensic toxicological analysis.
中文关键词	扎来普隆 ; 脱乙基扎来普隆 ; 超高效液相色谱-串联质谱 ; 固相萃取
英文关键词	Zaleplon Desethylzaleplon UPLC/MS/MS 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:5674811
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/234169
作者单位	1.中国人民公安大学, 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	徐多麒,王继芬,张蕾萍,等. 超高效液相色谱-三重四极杆质谱法检测血中脱乙基扎来普隆[J],2016,35(3):280-282.
APA	徐多麒,王继芬,张蕾萍,&林宽.(2016).超高效液相色谱-三重四极杆质谱法检测血中脱乙基扎来普隆.分析试验室,35(3),280-282.
MLA	徐多麒,et al."超高效液相色谱-三重四极杆质谱法检测血中脱乙基扎来普隆".分析试验室 35.3(2016):280-282.