超声波辅助酶提取结合高效液相色谱-电感耦合等离子体质谱法测定富硒蔬菜中硒形态  

Determination of selenium species in selenium-enriched vegetables by high performance liquid chromatography-inductively coupled plasma-mass spectrometry after ultrasonic-assisted extraction with enzyme

作　　者：李倩 刘兴勇[1] 陈兴连[1] 罗兰 尹本林[1] 李新宇 杜丽娟[1] 王云美[1] LI Qian;LIU Xingyong;CHEN Xinglian;LUO Lan;YIN Benlin;LI Xinyu;DU Lijuan;WANG Yunmei(Institute of Agricultural Quality Standard&Testing Technique,Yunnan Academy of Agricultural Sciences,Kunming 650205,China;Yunnan Institute of Product Quality Supervision&Inspection,Kunming 650223,China)

机构地区：[1]云南省农业科学院质量标准与检测技术研究所,云南昆明650205 [2]云南省产品质量监督检验研究院,云南昆明650223

出　　处：《食品与发酵工业》2024年第2期306-311,共6页Food and Fermentation Industries

基　　金：云南省重大科技专项(农业)(202102AE090051-1-01)。

摘　　要：该研究建立了利用高效液相色谱-电感耦合等离子体质谱法(high performance liquid chromatography-inductively coupled plasma-mass spectrometry,HPLC-ICP-MS)同时测定富硒蔬菜中SeO_(4)^(2-)、SeO_(3)^(2-)、SeMet、SeCys 2、MeSeCys等5种硒形态化合物含量的方法。蔬菜样品0.2 g加入4 mg蛋白酶XIV,加入5.00 mL pH为7.5的水溶液在37℃超声波提取80 min,微孔滤膜过滤,利用Hamilton PRP-X100阴离子交换柱,以25 mmol/L柠檬酸溶液(pH 6.0)为流动相,可在7 min内完成5种硒形态的完全分离。SeO_(4)^(2-)、SeO_(3)^(2-)、SeMet、SeCys 2、MeSeCys的线性相关系数为0.9993~0.9995,回收率范围为96.3%~104.2%,相对标准偏差小于7.6%。实验结果表明该法操作简便、快速、精密度及准确度良好,适用于富硒蔬菜中硒的形态分析。This study established a method to simultaneously detect the concentration of SeO_(4)^(2-),SeO_(3)^(2-),SeMet,SeCys_(2)and MeSeCys in selenium-enriched vegetables by high performance-inductively coupled plasma-mass spectrometry(HPLC-ICP-MS).Add 4 mg protease XIV and 5 mL aqueous solution with pH 7.5 in 0.2 g sample,treat with ultrasound at 37℃for 80 min,the supernatant pass through 0.22μm filter membrane.The five selenium species were separated completely within 7 min by Hamilton PRP-X100 anion exchange column under the condition of mobile phase 25 mmol/L citric acid(pH=6.0).The linear coefficients of five selenium species were between 0.9993 to 0.9995,and the recoveries of the spiked samples ranged from 96.3%to 104.2%,with the RSD below 7.6%.This method is simple,rapid,precision and accurate,it is thus suitable for the analysis of selenium species in selenium-enriched vegetables.

关 键 词：高效液相色谱-电感耦合等离子体质谱法 硒形态 富硒蔬菜 

分 类 号：TS255.7[轻工技术与工程—农产品加工及贮藏工程] O657.63[轻工技术与工程—食品科学与工程]