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	超高效液相色谱-串联质谱法同时测定血液中5种乌头类生物碱
其他题名	Simultaneous Determination of 5 Aconitum Alkaloids in Bloods by UHPLC-MS/MS
	滕傲雪 1; 王瑞花 2; 何洪源 1; 常靖 2
来源期刊	理化检验. B, 化学分册
ISSN	1001-4020
出版年	2018
卷号	54 期号:8 页码:941-945
中文摘要	采用超高效液相色谱-串联质谱法同时测定血液中乌头碱、次乌头碱、新乌头碱、滇乌头碱和雪上一枝蒿甲素等5种乌头类生物碱的含量。在1 mL血液样品中加入0.1 mol · L~(-1)盐酸溶液4 mL,振荡10 min,以8 000 r · min~(-1)转速离心30 min,上清液经Waters Oasis MCX固相萃取柱净化。以ACQUITY UPLC BEH C_(18)色谱柱为分离柱,以不同体积比的乙腈和水(用氨水调pH至10)的混合液为流动相进行梯度洗脱,质谱分析中采用电喷雾离子源(正离子扫描)和多反应监测模式。5种乌头类生物碱的质量浓度均在1.0~200 g· L~(-1)内与其对应的峰面积呈线性关系,方法的检出限(3S/N)为0.1~0.5 g · L~(-1)。以空白样品为基体进行加标回收试验,所得回收率为75. ~115%,测定值的相对标准偏差(n=6)为1.3%~6.5%。
英文摘要	UHPLC-MS/MS was applied to the simultaneous determination of 5 aconitum alkaloids, i. e. aconitine,hypaconitine,mesaconitine,yunaconitine and bullatine A in bloods. The blood sample (1 mL) was oscillated in 0.1 mol · L~(-1) hydrochloric acid solution (4 mL) for 10 min, and then was centrifuged at the speed of 8 000 r · min~(-1) for 30 min. The supernatant was purified with Waters Oasis MCX solid phase extraction column. ACQUITY UPLC BEH C_(18) chromatographic column was used as stationary phase, and the mixture of acetonitrile and water (pH was adjusted to 10 with ammonia) mixed in different ratios was used as mobile phase in gradient elution. ESI~+ and multi-reactions monitor mode were adopted in MS/MS. Linear relationships between values of peak area and mass concentration of the 5 aconitum alkaloids were kept in the same range of 1.0 - 200 g · L~(-1), with detection limits (3S/N) in the range of 0.1-0.5 g · L~(-1). On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 75.6%-115%, with RSDs (n= 6) in the range of 1.3% -6.5%.
中文关键词	超高效液相色谱-串联质谱法 ; 乌头类生物碱 ; 血液
英文关键词	UHPLC-MS/MS aconitum alkaloid blood
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:6313085
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/237912
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	滕傲雪,王瑞花,何洪源,等. 超高效液相色谱-串联质谱法同时测定血液中5种乌头类生物碱[J],2018,54(8):941-945.
APA	滕傲雪,王瑞花,何洪源,&常靖.(2018).超高效液相色谱-串联质谱法同时测定血液中5种乌头类生物碱.理化检验. B, 化学分册,54(8),941-945.
MLA	滕傲雪,et al."超高效液相色谱-串联质谱法同时测定血液中5种乌头类生物碱".理化检验. B, 化学分册 54.8(2018):941-945.