基于反相色谱-电感耦合等离子体质谱联用技术快速测定饲料中砷形态的研究
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摘要
建立了反相高效液相色谱-电感耦合等离子体质谱联用技术(RHPLC-ICP-MS)测定饲料中砷酸盐砷[As(Ⅴ)]、一甲基砷酸(MMA)、亚砷酸盐[As(Ⅲ)]、二甲基砷酸(DMA)、甜菜碱(AsB)的分析方法。饲料样品经硝酸溶液(10+990)提取,结合Agilent ZORBAX SB-Aq反相色谱柱(4.6 mm×250 mm,5μm),在5 min内完成5种砷形态物质的分离和检测。结果表明:各形态砷在1～50 ng/mL范围内线性良好(R>0.999),检出限为0.258～1.150 ng/mL,加标回收率在83.6%～113.1%之间,相对标准偏差(RSD)均小于5%。通过实际样品检测,该方法适用于饲料中主要砷形态物质的快速定量分析。
A method was developed for the simultaneous determination of arsenic acid [As(Ⅴ)], monomethylarsonic acid(MMA), arsenious acid [As(Ⅲ)], dimethylasinic acid(DMA) and arsenobetaine(AsB) in feed by reversed high phase liquid chromatography-inductively couple plasma-mass spectrometry(RHPLC-ICP-MS). Feed samples were extracted with nitric acid solution(10+990), and five arsenic species in feed sample were separated and detected by Agilent ZORBAX SB Aq reversed-phase column(4.6 mm×250 mm, 5 μm) within 5 minutes. The results showed that the linearity of arsenic speciation was good in the range of 1 ng/mL～50 ng/mL(R>0.999), the detection limit was 0.258 ng/mL～1.150 ng/mL, the recovery rate was between 83.6% and 113.1%, and the relative standard deviation(RSD) was less than 5%. The method was suitable for the detection of main arsenic speciation in feed through testing the actual samples.
A method was developed for the simultaneous determination of arsenic acid [As(Ⅴ)], monomethylarsonic acid(MMA), arsenious acid [As(Ⅲ)], dimethylasinic acid(DMA) and arsenobetaine(AsB) in feed by reversed high phase liquid chromatography-inductively couple plasma-mass spectrometry(RHPLC-ICP-MS). Feed samples were extracted with nitric acid solution(10+990), and five arsenic species in feed sample were separated and detected by Agilent ZORBAX SB Aq reversed-phase column(4.6 mm×250 mm, 5 μm) within 5 minutes. The results showed that the linearity of arsenic speciation was good in the range of 1 ng/mL～50 ng/mL(R>0.999), the detection limit was 0.258 ng/mL～1.150 ng/mL, the recovery rate was between 83.6% and 113.1%, and the relative standard deviation(RSD) was less than 5%. The method was suitable for the detection of main arsenic speciation in feed through testing the actual samples.
引文
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[6]王博,张浩然,陆淳,等.高效液相色谱-电感耦合等离子体-串联质谱法同时测定饲料中As(Ⅲ)、As(Ⅴ)、氨苯胂酸和洛克沙胂[J].分析科学学报,2018(1):100-104.
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[9]韩枫,岳兵,米健秋,等.反相色谱-电感耦合等离子体质谱联用技术快速测定大米中无机砷[J].环境化学,2015(1):194-197.
[10]宋睿,宋娟娥,贠照军.反相色谱-电感耦合等离子体质谱法快速测定大气颗粒物中的无机砷[J].环境化学,2017,36(1):198-200.
[11]国家卫生和计划生育委员会.食品安全国家标准食品中总砷和无机砷的测定:GB5009.11-2014[S].北京:中国标准出版社,2014.
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[14]国家质量监督检验检疫总局.食品中无机砷的测定液相色谱-电感耦合等离子体质谱法:GB23372-2009[S].北京:中国标准出版社,2009.
[2]Aposhian H V,Aposhian M M.Arsenic Toxicology:Five Questions[J].Chemistry Research in Toxicology,2006,19(1):1-15.
[3]Mcsheehy S,Szpunar J,Morabito R,et al.The speciation of arsenic in biological tissues and the certification of reference materials for quality control[J].Trends in Analytical Chemistry,2003,22(4):191-209.
[4]潘雨齐,李时卉,彭亮,等.环境中砷元素的分布、化学形态、生物毒性及其污染治理[J].农业环境与发展,2012,29(3):64-67.
[5]陈国,吴银良.应用HPLC-ICP-MS联用法分析饲料中As的四种形态[J].安徽农学通报,2017(6):165-168.
[6]王博,张浩然,陆淳,等.高效液相色谱-电感耦合等离子体-串联质谱法同时测定饲料中As(Ⅲ)、As(Ⅴ)、氨苯胂酸和洛克沙胂[J].分析科学学报,2018(1):100-104.
[7]许锦华.高效液相色谱-电感耦合等离子体质谱联用法测定饲料中的无机砷及其他砷形态[J].饲料工业,2017,38(17):43-46.
[8]巩佳第,曹晓林,曹赵云,等.液相色谱-电感耦合等离子体质谱法测定稻米中的5种砷形态[J].色谱,2014(7):717-722.
[9]韩枫,岳兵,米健秋,等.反相色谱-电感耦合等离子体质谱联用技术快速测定大米中无机砷[J].环境化学,2015(1):194-197.
[10]宋睿,宋娟娥,贠照军.反相色谱-电感耦合等离子体质谱法快速测定大气颗粒物中的无机砷[J].环境化学,2017,36(1):198-200.
[11]国家卫生和计划生育委员会.食品安全国家标准食品中总砷和无机砷的测定:GB5009.11-2014[S].北京:中国标准出版社,2014.
[12]国家食品药品监督管理总局.食品安全国家标准食品中多元素的测定:GB 5009.268-2016[S].北京:中国标准出版社,2016.
[13]国家质量监督检验检疫总局.饲料中兽药及其他化学物检测试验规程:GB/T 23182-2008[S].北京:中国标准出版社,2008.
[14]国家质量监督检验检疫总局.食品中无机砷的测定液相色谱-电感耦合等离子体质谱法:GB23372-2009[S].北京:中国标准出版社,2009.