摘要
采用高效液相色谱-电感耦合等离子体质谱(HPLC-ICPMS)法测定富硒山茶油中硒代胱氨酸、甲基-硒代半胱氨酸、亚硒酸根、硒代蛋氨酸、硒酸根5种硒形态化合物含量。样品0.5 g经蛋白酶K和超声提取,利用Hamilton PRP-X100色谱柱进行分离,以5 mmol/L柠檬酸溶液(pH 5.5)、超纯水为流动相进行梯度洗脱,外标法定量。结果表明,采用1 mL蛋白酶K溶液为提取剂,超声提取50 min,5种硒化合物在15 min内得到了有效分离。5种硒化合物的质量浓度为5.0~100μg/L时,线性关系良好,相关系数均大于0.999,检出限为0.16~1.15μg/L,定量限为9.6~69.0μg/kg,相对标准偏差(RSD)为1.86%~4.87%,样品加标回收率为94.6%~113.1%。
The contents of 5 selenium species(SeCys_2,SeMC,Se(Ⅳ),SeMet,and Se(Ⅵ)) in selenium enriched camellia oil were determined by HPLC-ICP-MS.Sample 0.5 g was extracted with protease K and ultrasound,separated by Hamilton PRP-X100 column.Mobile phases were 5 mmol/L citric acid(pH 5.5) aqueous solution and ultra-pure water for gradient elution.Quantification was performed by the external standard method.The results indicated that,5 selenium compounds were ultrasonically extracted by using 1mL of protease K(10 mg/mL) for 50 minutes,and then,separated with gradient elution in 15 min.When the mass concentration of 5 selenium species were 5.0-100.0 μg/L,the linear relationship was good,the correlation coefficient was larger than 0.999,and the limits of detection were in the range of 0.16-1.15 μg/L,the limits of quantitation were 9.6-69.0 μg/kg.The relative standard deviation(RSD) of precision were 1.86%-4.87%,and the standard recovery were 94.6%-113.1%.
作者
刘文政
贾亚琪
周贻兵
毕珊
刘利亚
Liu Wenzheng;Jia Yaqi;Zhou Yibing;Bi Shan;Liu Liya(Guizhou Center for Diseases Control and Prevention,Guiyang 550004;Guizhou Academy of Environmental Science and Designing,Guiyang 550081)
出处
《中国粮油学报》
CSCD
北大核心
2023年第9期197-203,共7页
Journal of the Chinese Cereals and Oils Association
基金
贵州省卫生健康委科学技术基金项目(gzwkj2022-208)
贵州省疾病预防控制中心科学(青年)技术基金项目(2021-E1-2青)。
关键词
HPLC-ICP-MS
富硒山茶油
硒
形态分析
超声提取
HPLC-ICP-MS
selenium enriched camellia oil
selenium
speciation analysis
ultrasonic extraction
作者简介
第一作者:刘文政,男,1988年出生,主管技师,食品及食品相关产品分析研究,lwzjyq1988@163.com;通信作者:刘利亚,男,1978年出生,主任技师,食品安全及风险预警方面的研究,541767047@qq.com。
