超声辅助提取结合高效液相色谱-电感耦合等离子体质谱联用技术测定牛蒡和三七中硒形态

Determination of Selenium Species in Burdock and Panax Notoginseng Using Ultrasonic Assistant Extraction Combined with High Performance Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry

用蛋白酶K和脂肪酶作为提取剂、用超声波辅助提取牛蒡和三七样品中的硒形态。建立了高效液相色谱-电感耦合等离子体质谱联用技术测定牛蒡和三七样品中硒代胱氨酸（Se Cys2）、亚硒酸盐[Se？]、硒代蛋氨酸（Se Met）和硒酸盐[Se？]的新方法。用8 mmol/L p H 5.0的柠檬酸作为流动相,在8 min内可分离4种硒形态。利用CH4作为DRC反应气体,可消除了40Ar40Ar＋对80Se＋的干扰,提高了准确度。Se Cys2、Se？、SeMet和Se？的检出限分别为0.088,0.033,0.30和0.17 ng/m L,相关系数（R2）均大于0.9995,加标回收率范围为95.1%~114.6%,RSD〈3%。将本方法应用于牛蒡和三七中硒形态分析,结果令人满意。

A high performance liquid chromatography-inductively coupled plasma mass spectrometric （HPLC- ICP-MS） method for analysis of selenocystine （SeCys2）, selenite （Se（Ⅳ））, selenomethionine （SeMet） and selenate （Se （VD） was described. Chromatographic separation was performed using 8 mmol/L citric acid solution （ pH 5 ）. The potentially interfering 40Ar40Ar＋ at selenium masses of m/z 80 was reduced using CH4 as a reactive cell gas in the dynamic reaction cell. The selenium species was extracted using ultrasonic extraction system with a mixture of protease K and lipase. The limits of detection for SeCys2, Se（Ⅳ）, SeMet, and Se（Ⅵ） were observed as 0. 088, 0. 033 , 0. 30, and 0.17 ng/mL, respectively. The correlation coefficients were greater than 0. 9995. The recoveries were observed in the range of 95.1%-114.6%. The developed method was successfully applied for the determination of selenium species in Burdock and Panax notoginseng.