摘要
目的建立液质联用(liquid chromatography-mass spectrometry,LC-MS)定量分析测定大蒜提取物中S-烯丙基-L-半胱氨酸的方法。方法采用LC-MS法检测,ZORBAX Eclipse XDB-C8(4.6 mm×250 mm,5μm)色谱柱,流动相组成:1‰甲酸水-甲醇(95∶5),流速:0.8 mL/min;柱后分流检测,分流比2∶1;柱温:25℃;ESI电离源:负离子检测模式;干燥气流速:10.0 L/min;雾化室压力:30 psig;干燥气温度:350℃。选择离子方式检测(SI M):S-烯丙基-L-半胱氨酸m/z160和S-烯丙基-L-半胱氨酸亚砜m/z176。结果S-烯丙基-L-半胱氨酸在0.062 5～2μg/mL浓度范围内线性关系良好,检测限0.01μg/mL,日内RSD4.11%、日间RSD4.49%,方法平均回收率为101.63%。结论此方法简单、准确,适于分析测定大蒜提取物中S-烯丙基-L-半胱氨酸的含量,并且测得该提取物中S-烯丙基-L-半胱氨酸的平均含量为0.514μg/mg。
Objective To develop a liquid chromatography-mass spectrometry（LC-MS） method for the determination of S-allyl-L-cystein in extraction of garlic. Methods A LC-MS method was established on a ZORBAX Eclipse XDB-C8（4.6 mm×250 mm,5 μm）column with the mobile phase consisting of 1‰ formic acid water-methanol（95∶5）,flow rate of 0.8 mL/min and detection with post-column splitting.The split ratio was 2∶1,column temperature was set at 25 ℃.The mass spectrometer equipped with ESI and the ion source was operated in negative mode.The dry gas flow was 10.0 L/min,the nebulizer pressure was 30 psig,and the vaporizer temperature was 350 ℃.SIM detector,S-allyl-L-cystein m/z 160 and S-allyl-L-cystein sulfoxide m/z 176. Results The calibration curves showed good linearity in the range of 0.062 5-2 μg/mL of S-allyl-L-cystein.The detection limit was 0.01 μg/mL.The within-day RSD was 4.11% and the day-to-day RSD was 4.49%.The average recovery for S-allyl-L-cystein was 101.63%. Conclusions The method is simple and accurate.It is adapted to determine and analyze S-allyl-L-cystein in extraction of garlic and the average content of S-allyl-L-cystein is 0.514 μg/mg.
出处
《复旦学报（医学版）》
CAS
CSCD
北大核心
2010年第1期68-70,87,共4页
Fudan University Journal of Medical Sciences
基金
上海市科学技术委员会联合-利华奖资助项目(08540750400)
