干旱区生态环境知识资源中心(Arid): 液相色谱-质谱法测定人尿中雷公藤新碱含量

Arid

	液相色谱-质谱法测定人尿中雷公藤新碱含量
其他题名	LC-MS Determination of Euonine in Human Urine
	沈称意 1; 施跃锦 1; 蔡美强 1; 金米聪 2
来源期刊	理化检验. B, 化学分册
ISSN	1001-4020
出版年	2013
卷号	49 期号:7 页码:773-776
中文摘要	提出了人尿中雷公藤新碱的液相色谱-质谱测定方法。尿液样品经WatersOasisMCX固相萃取柱富集并净化,萃取柱用含氨水的乙腈洗脱。洗脱液用ZorbaxPlusRRHDC18反相色谱柱(50mm*2.1mm,1.8mum),以乙酸盐缓冲溶液和乙腈(30+70)混合液为流动相进行分离,采用大气压化学电离源正离子模式在选择离子监测模式下进行检测,雷公藤新碱的定量离子为m/z806。雷公藤新碱的质量浓度在0.2~50.0mug.L~(-1)范围内与峰面积呈线性关系,测定下限(10S/N)为0.2mug·L~(-1)。回收率在84.5%~94.0%之间,日内(n=6)和日间(n=5)精密度分别小于7%和10%。
英文摘要	A method for the determination of euonine in human urine by LC-MS was proposed. Euonine in sample was separated. enriched and purified on Waters Oasis MCX SPE column. The SPE column was eluted with ammoniacal acetonitrile. The eluate was used for LC-MS determination. Zorbax Plus RRHD C_18 column(50 mm* 2.1 mm, 1.8 mum) was used as chromatographic column, and a mixture of acetate buffer solution and acetonitrile (30 + 70) was used as mobile phase in the separation. Atmospheric pressure chemical ionization source with positive ionization mode as well as selected ion monitoring mode was used in the detection. Quantitative ion of euonine used was m/z 806. Linear relationship between values of peak area and mass concentration of euonine was kept in the range of 0.250.0 mug·L~(-1), with lower limit of determination (10S/N) of 0.2 mug·L~(-1). Values of recovery were ranged from 84.5% to 94.0%. Values of intraday RSD’s (n = 6) and interday RSD’s (n=5) found were less than 7% and 10%, respectively.
中文关键词	液相色谱-质谱法 ; 固相萃取 ; 雷公藤新碱 ; 尿液
英文关键词	LC-MS Solid-phase extraction Euonine Urine
语种	中文
国家	中国
收录类别	CSCD
WOS类目	CHEMISTRY ANALYTICAL
WOS研究方向	Chemistry
CSCD记录号	CSCD:4919934
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/229839
作者单位	1.浙江工商大学环境科学与工程学院, 杭州, 浙江 310035, 中国; 2.宁波市疾病预防控制中心, 宁波市毒物研究与控制重点实验室, 宁波, 浙江 315010, 中国
推荐引用方式 GB/T 7714	沈称意,施跃锦,蔡美强,等. 液相色谱-质谱法测定人尿中雷公藤新碱含量[J],2013,49(7):773-776.
APA	沈称意,施跃锦,蔡美强,&金米聪.(2013).液相色谱-质谱法测定人尿中雷公藤新碱含量.理化检验. B, 化学分册,49(7),773-776.
MLA	沈称意,et al."液相色谱-质谱法测定人尿中雷公藤新碱含量".理化检验. B, 化学分册 49.7(2013):773-776.