干旱区生态环境知识资源中心(Arid): 固相萃取纯化-高效液相色谱-串联质谱法测定尿液中痕量雷公藤红素

Arid

	固相萃取纯化-高效液相色谱-串联质谱法测定尿液中痕量雷公藤红素
其他题名	HPLC-MS/MS Determination of Trace Amount of Celastrol in Urine After Purification with Solid-Phase Extraction
	陈晓红 1; 欧阳小琨 2; 金米聪 1
来源期刊	理化检验. B, 化学分册
ISSN	1001-4020
出版年	2010
卷号	46 期号:8 页码:948-951
中文摘要	提出了尿液中雷公藤红素的高效液相色谱-串联质谱测定方法. 尿液样品经Waters Oasis~R HLB固相萃取柱富集、净化后,以XDB C_(18)反相色谱柱(150 mm*4.6 mm,5mum)为分离柱,以0.5 g·L~(-1)乙酸-乙腈(25+75)混合溶液为流动相,以氢化可的松为内标,采用负离子模式大气压化学电离源在多反应监测模式下进行检测,雷公藤红素和内标的定量离子对分别为m/z449/405和m/z419/329. 线性范围为0.2~50.0mug·L~(-1),检出限(3S/N)为0.07mug·L~(-1). 日内精密度(n=6)和日间精密度(n=15)分别小于9.3%和11.4%
英文摘要	A method for the determination of celastrol in urine by high-performance liquid chromatography hyphenated with tandem mass spectrometry (HPLC-MS/MS) was proposed. Celastrol in samples was enriched and purified on Waters Oasis~R HLB SPE column. The eluate was used for HPLC-MS/MS determination, in which the XDB C_(18) reserved-phase column (150 mm*4.6 mm, 5mum) was used as chromatographic column, and a mixture of 0.5 g·L~(-1)acetic acid solution and acetonitrile (25+75) was used as mobile phase. Hydrocortisone was used as internal standard. Abnospheric pressure chemical ionization source with negative ionization mode as well as multiple reaction monitoring mode was used in the detection. Ion pairs used for the quantitative analysis werem/z449/405 for celastrol andm/z419/329 for internal standard. Linearity range was found between 0.2-50.0mug·L~(-1), and the detection limit (3S/N) found was 0.07mug·L~(-1). Values of RSD′s of intra-day (n=6) and inter-day (n=15) found were less than 9.3% and 11.4%, respectively
中文关键词	高效液相色谱-串联质谱法 ; 雷公藤红素 ; 固相萃取 ; 尿液
英文关键词	HPLC-MS/MS Celastrol Solid-phase extraction 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:3984775
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/225361
作者单位	1.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; 2.浙江海洋学院食品与药学院, 舟山, 浙江 316004, 中国
推荐引用方式 GB/T 7714	陈晓红,欧阳小琨,金米聪. 固相萃取纯化-高效液相色谱-串联质谱法测定尿液中痕量雷公藤红素[J],2010,46(8):948-951.
APA	陈晓红,欧阳小琨,&金米聪.(2010).固相萃取纯化-高效液相色谱-串联质谱法测定尿液中痕量雷公藤红素.理化检验. B, 化学分册,46(8),948-951.
MLA	陈晓红,et al."固相萃取纯化-高效液相色谱-串联质谱法测定尿液中痕量雷公藤红素".理化检验. B, 化学分册 46.8(2010):948-951.