干旱区生态环境知识资源中心(Arid): 超高效液相色谱-串联质谱法测定保健食品中10种磷酸二酯酶-5抑制剂

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	超高效液相色谱-串联质谱法测定保健食品中10种磷酸二酯酶-5抑制剂
其他题名	Simultaneous Determination of Ten Phosphodiesterase-5Inhibitors in Health Foods by Ultra Performance Liquid Chromatography with Tandem Mass Spectrometry
	勾新磊; 赵新颖; 高峡; 周明强; 刘伟丽
来源期刊	质谱学报
ISSN	1004-2997
出版年	2016
卷号	37 期号:6 页码:554-561
中文摘要	建立了超高效液相色谱-串联质谱法(UPLC-MS/MS)同时测定保健食品中10种磷酸二酯酶-5(PDE-5)抑制剂。样品采用Waters Acquity UPLC BEH C18(100 mm2.1 mm1.7mum)色谱柱分离,以甲醇-0.1%甲酸水溶液为流动相进行梯度洗脱,甲醇为提取溶剂超声萃取,经HLB固相萃取柱净化浓缩;在电喷雾正离子模式下,以多反应监测(MRM)模式进行检测。结果表明,10种磷酸二酯酶-5抑制剂在1.0~100.0mug/L范围内线性关系良好,线性相关系数(R2)均大于0.993,方法定量限为1.0mug/kg;空白样品在100.0、200.0和1 000.0mug/kg添加水平下的回收率为85.6%~94.3%。该方法简便、快速、检出限低,适用于保健食品中10种磷酸二酯酶-5抑制剂的同时检测。
英文摘要	A method was developed for simultaneous determination of ten phosphodiesterase- 5(PDE-5)inhibitors in health foods by ultra performance liquid chromatographytandem mass spectrometry(UPLC-MS/MS),such as vardenafil,acetildenafil,sildenafil, homosildenafil,udenafil,tadalafil,thioaildenafil,gendenafil,pseudovarnafil,nor neosildenafil.The separation was performed using water containing 0.1%formic acid and methanol as mobile phases with gradient elution at a flow rate of 0.2 mL/min. Qualitative and quantitative analysis were achieved after the chromatographic separation on a Waters Acquity UPLC BEH C18 column(100 mm2.1 mm1.7mum).The electrospray ionization(ESI)source in positive ion mode was used for analysis of ten phosphodiesterase- 5 inhibitors in the multiple reaction monitoring(MRM)mode.The nuclear ratio of parent ion and daughter ion,cone voltage,collision voltage were investigated. The sample was ultrasonic-assisted treatment using the methanol as extraction solvent, and then purified by Waters Oasis HLB solid-phase extraction (SPE)column. The results indicate that the linear range of the method is from 1.0mug/L to 100.0mug/L with R2>0.993,which means the method has a good linearity.The limits of detection(LOD)and limits of quantification(LOQ)of ten phosphodiesterase-5 inhibitors are 0.3-1.0mug/kg and 1.0-2.5mug/kg,respectively.The average recoveries of ten phosphodiesterase- 5 inhibitors at three spiked levels of 100.0,200.0 and 1 000.0mug/kg are 85.6%- 94.3%.The method was applied to analysis of the investigated compounds in twenty health foods.The results indicate that sildenafil are found in eighteen samples with the range of 1.3-210.8 mg/g,vardenafil and tadalafil are found in a tablet and a capsule, respectively.This method is accurate,simple,rapid and feasible for simultaneous determination of phosphodiesterase-5inhibitors in health foods.
中文关键词	超高效液相色谱-串联质谱(UPLC-MS/MS) ; 磷酸二酯酶-5抑制剂(PDE-5) ; 固相萃取 ; 保健食品
英文关键词	ultra performance liquid chromatography-tandem mass spectrometry(UPLCMS/ MS) phosphodiesterase-5inhibitors(PDE-5) solid phase extraction health foods
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:5860811
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/235317
作者单位	北京市理化分析测试中心, 有机材料检测技术与质量评价北京市重点实验室, 北京 100089, 中国
推荐引用方式 GB/T 7714	勾新磊,赵新颖,高峡,等. 超高效液相色谱-串联质谱法测定保健食品中10种磷酸二酯酶-5抑制剂[J],2016,37(6):554-561.
APA	勾新磊,赵新颖,高峡,周明强,&刘伟丽.(2016).超高效液相色谱-串联质谱法测定保健食品中10种磷酸二酯酶-5抑制剂.质谱学报,37(6),554-561.
MLA	勾新磊,et al."超高效液相色谱-串联质谱法测定保健食品中10种磷酸二酯酶-5抑制剂".质谱学报 37.6(2016):554-561.