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LC-ICP-MS法同时测定富硒大米中有机硒和无机砷

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采用液相色谱-电感耦合等离子体质谱(LC-ICP-MS)技术,建立富硒大米中有机硒和无机砷同时检测的方法,用于检测湖北省市售富硒大米中有机硒和无机砷的含量。富硒大米前处理方法选用15 mg蛋白酶E和15 mg蛋白酶K混合提取,色谱条件采用Aglient ZORBAX SB-Aq色谱柱,流动相为20 mmol/L柠檬酸溶液+5 mmol/L己烷磺酸钠溶液+1%甲醇溶液(pH=4。0),1 mL/min流速进样,质谱采用HEHe模式,可在5 min内完全分离出3种有机硒和2种无机砷。3种有机硒和2种无机砷在1~50 μg/L范围内具有良好的线性关系,相关系数(R2)均大于0。999 0,As(Ⅴ)、As(Ⅲ)、SeCys2、MeSeCys、SeMet的检出限分别为0。10、0。12、0。18、0。15、0。15 μg/L,满足检测要求。无机砷的回收率为96。2%~101。3%,相对标准偏差为2。5%~3。9%,有机硒的回收率为72。4%~100。6%,相对标准偏差为2。1%~4。1%。该方法操作简便、快速、灵敏度高,可用于富硒大米中有机硒和无机砷的同时检测。
Simultaneous determination of organic selenium and inorganic arsenic in selenium rich rice by LC-ICP-MS method
Using liquid chromatography inductively coupled plasma mass spectrometry(LC-ICP-MS)technology,a method for simul-taneous detection of organic selenium and inorganic arsenic in selenium-rich rice had been established,which was used to detect the content of organic selenium and inorganic arsenic in selenium-rich rice sold in Hubei Province.The pre-treatment method for seleni-um rich rice involved the mixed extraction by using of 15 mg proteinase E and 15 mg proteinase K,the chromatographic conditions were performed using an AgClient ZORBAX SB Aq column,and the mobile phase consistd of a 20 mmol/L citric acid solution,a 5 mmol/L sodium hexane sulfonate solution,and a 1%methanol solution(pH=4.0).Sample in jection was conducted at a flow rate of 1 mL/min,mass spectrometry used HEHe mode,and three types of organic selenium and two types of inorganic arsenic were separated completely within 5 minutes.The three types of organic selenium and two types of inorganic arsenic showed a good linear relationship ranging from 1 to 50 μg/L,with correlation coefficients(R2)greater than 0.999 0;the detection limits of As(Ⅴ),As(Ⅲ),SeCys2,MeSeCys,and SeMet were 0.10,0.12,0.18,0.15,and 0.15 μg/L,respectively,which met the detection requirements.The recovery rate of inorganic arsenic was 96.2%~101.3%,with a relative standard deviation of 2.5%~3.9%;the recovery rate of organic selenium was 72.4%~100.6%,with a relative standard deviation of 2.1%~4.1%.This method was easy to operate,fast,and highly sensitive,and could be used for simultaneous detection of organic selenium and inorganic arsenic in selenium rich rice.

selenium rich riceorganic seleniuminorganic arsenicLC-ICP-MS method

苏莹、林津、冯灏、李越、郭青青、周陶鸿

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湖北省食品质量安全监督检验研究院/国家市场监管重点实验室/动物源性食品中重点化学危害物检测技术/湖北省食品质量安全检测工程技术研究中心/湖北时珍实验室,武汉 430075

富硒大米 有机硒 无机砷 LC-ICP-MS法

2024

湖北农业科学
湖北省农业科学院 华中农业大学 长江大学 黄冈师范学院

湖北农业科学

CSTPCD
影响因子:0.442
ISSN:0439-8114
年,卷(期):2024.63(9)