摘要
目的建立大蒜中硒形态的高效液相色谱-电感耦合等离子体串联质谱测定方法。方法采用ZORBAX SB-Aq反相离子对色谱柱作为分析柱,10.00 mmol/L柠檬酸(铵)+5.00 mmol/L己烷磺酸钠+2.00%甲醇为流动相,梯度洗脱,可在10.00 min内完成对硒酸根(SeO_(4)^(2-))、亚硒酸根(SeO_(3)^(2-))、硒代胱氨酸(SeCys2)、甲基-硒代半胱氨酸(MeSeCys)、硒代蛋氨酸(SeMet)和硒代乙硫氨酸(SeEt)的分离分析。采用恒温振摇辅助酶提取法对大蒜进行提取。结果SeO_(4)^(2-)、SeO_(3)^(2-)、SeCys2、MeSeCys、SeMet和SeEt的方法检出限分别为0.40、0.40、0.44、0.47、0.35和0.45μg/kg,0.00~100.00μg/L范围内线性相关系数(r)均>0.999,线性关系良好。除SeCys2,加标回收率为79.00%~104.00%,相对标准偏差为2.20%~5.00%(n=7)。结论该方法稳定性好,灵敏度和准确度高,适用于大蒜中5种硒形态分析。
Objective To establish a method for the determination of selenium species in Se-enriched garlic with high performance liquid chromatography-inductively coupled plasma tandem mass spectrometry(HPLC-ICP-MS/MS).Methods ZORBAX SB-Aq column was used as analytical column;10 mmol/L citric acid(ammonium citrate),5 mmol/L sodium hexane sulfonate and 2%methanol were used as mobile phase for gradient elution.Baseline separation of selenate(SeO_(4)^(2-)),selenite(SeO_(3)^(2-)),selenocysteine(SeCys2),methylselenocysteine(MeSeCys),selenomethionine(SeMet)and Selenoethionine(SeEt)were completed in 10 min.Constant temperature oscillating assisted enzyme extraction was used to extract selenium species in garlic samples.Results The detection limits for SeO^(2-)_(4),SeO_(3)^(2-),SeCys2,MeSeCys,SeMet and SeEt were 0.40,0.40,0.44,0.47,0.35 and 0.45μg/kg,respectively.The linear correlation coefficients(r)were all above 0.999 in the range of 0-100.0μg/L.Except SeCys2,the recoveries were between 79.0%-104.0%and the relatives standard deviations were within 2.2%-5.0%.Conclusion The result showed that the method had good stability with high sensitivity and accuracy,and was suitable for determination of five selenium species in garlic.
作者
张珂
张钦龙
张蜀
张幔玲
高舸
ZHANG Ke;ZHANG Qinlong;ZHANG Shu;ZHANG Manling;GAO Ge(Chengdu Center for Disease Control and Prevention,Sichuan Chengdu 610041,China)
出处
《中国食品卫生杂志》
CSCD
北大核心
2021年第5期577-582,共6页
Chinese Journal of Food Hygiene
关键词
高效液相色谱-电感耦合等离子体串联质谱
富硒
大蒜
硒形态
酶提取
High performance liquid chromatography-inductively coupled plasma tandem mass spectrometry
Se-enriched
garlic
selenium species
enzyme extraction
