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

摘要

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( SeCys2)、亚硒酸盐[ SeⅣ]、硒代蛋氨酸(SeMet)和硒酸盐[SeⅥ]的新方法。用8 mmol/L pH 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40 Ar40 Ar+对80 Se+的干扰,提高了准确度。 SeCys2、SeⅣ、SeMet和SeⅥ的检出限分别为0.088,0.033,0.30和0.17 ng/mL,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 (SeⅣ), selenomethionine (SeMet) and selenate ( SeⅥ) 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 , SeⅣ, SeMet, and SeⅥwere 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.