加速溶剂萃取联合高效液相色谱-电感耦合等离子体质谱法测定畜肉制品中的6种砷形态
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摘要
采用高效液相色谱联用电感耦合等离子体质谱法(ICP-MS)测定畜肉制品中的一甲基砷、二甲基砷、三价砷、五价砷、砷甜菜碱和砷胆碱。称取经组织粉碎机粉碎的样品约3.0g置于不锈钢萃取池中,加入6g石英砂,搅拌均匀,以甲醇(2+1)溶液为提取溶剂,进行加速溶剂萃取。提取完成后,将提取液用甲醇(2+1)溶液定容至100mL,经0.45μm滤膜过滤。采用Dionex IonPac AS-17色谱柱(250mm×4.0mm,10μm)分离滤液中的6种砷形态,以20mmol·L~(-1) NH_4HCO_3溶液为流动相在1.0mL·min~(-1)流量下进行洗脱,采用ICP-MS测定洗脱液中6种砷形态。结果表明:6种砷形态质量浓度均在0.5～50.0μg·L~(-1)内与对应的响应强度呈线性关系,检出限(3S/N)在0.15～0.24μg·kg~(-1)之间。加标回收率在86.0%～108%之间,测定值的相对标准偏差(n=6)在2.6%～3.9%之间。
A method of HPLC-ICP-MS was applied to the determination of methyl arsenic,dimethyl arsenic,arsenic(Ⅲ),arsenic(Ⅴ),arsenic choline and arsenic betaine in livestock products.About 3.0 g of the sample pulverized by a tissue pulverizer was added into a stainless steel extraction tank,and 6 g of quartz sand was added.The mixture was stirred uniformly,and methanol(2+1) solution was used as extraction solvent to carry out accelerated solvent extraction.After the extraction was completed,the extract was made up to 100 mL with methanol(2+1) solution,and filtered through a 0.45μm filter membrane.The 6 arsenic species were seperated on a Dionex IonPac AS-17 column(250 mm×4.0 mm,10μm),with 20 mmol·L~(-1) NH_4HCO_3 solution as mobile phase for elution at a flow rate of 1.0 mL·min~(-1).ICP-MS was used to determine the 6 arsenic species in the eluate.The result showed that linear relationships were found between response intensity and mass concentration of the 6 arsenic species in the same range of 0.5-50.0μg·L~(-1),with detection limits(3 S/N) in the range 0.15-0.24μg·kg~(-1).Values of recovery obtained by standard addition method were in the range of 86.0%-108%,and RSDs(n=6) were in the range of 2.6%-3.9%.
A method of HPLC-ICP-MS was applied to the determination of methyl arsenic,dimethyl arsenic,arsenic(Ⅲ),arsenic(Ⅴ),arsenic choline and arsenic betaine in livestock products.About 3.0 g of the sample pulverized by a tissue pulverizer was added into a stainless steel extraction tank,and 6 g of quartz sand was added.The mixture was stirred uniformly,and methanol(2+1) solution was used as extraction solvent to carry out accelerated solvent extraction.After the extraction was completed,the extract was made up to 100 mL with methanol(2+1) solution,and filtered through a 0.45μm filter membrane.The 6 arsenic species were seperated on a Dionex IonPac AS-17 column(250 mm×4.0 mm,10μm),with 20 mmol·L~(-1) NH_4HCO_3 solution as mobile phase for elution at a flow rate of 1.0 mL·min~(-1).ICP-MS was used to determine the 6 arsenic species in the eluate.The result showed that linear relationships were found between response intensity and mass concentration of the 6 arsenic species in the same range of 0.5-50.0μg·L~(-1),with detection limits(3 S/N) in the range 0.15-0.24μg·kg~(-1).Values of recovery obtained by standard addition method were in the range of 86.0%-108%,and RSDs(n=6) were in the range of 2.6%-3.9%.
引文
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[12] 林琳,张素静,徐渭聪,等.血液和尿液中砷形态化合物的HPLC-ICP-MS分析[J].法医学杂志,2018,34(1):37-43.
[2] 程晓宏,杨清华,陈峰,等.食品安全中重金属检测方法的研究进展[J].江苏预防医学,2015,26(3):56-58.
[3] 周岩民,杜文兴,韩兆玉,等.洛克沙对肉鸭生产性能和砷残留及组织病变的影响[J].南京农业大学学报,2001,24(4):46-50.
[4] 王帅,邹勇平,周元元.超声辅助提取氢化物发生原子荧光法测定鹅肉中无机砷[J].分析与监测,2013,32(7):131-134.
[5] 陈玎玎,葛高飞.液相色谱-氢化物发生原子荧光光谱测定鸡肉中4种形态砷化合物[J].安徽农业大学学报,2017,22(3):388-391.
[6] 高鹭,董伟峰,彭心婷,等.高效液相色谱氢化物发生原子荧光光谱联用检测海藻中砷形态[J].食品安全质量检测学报,2015,6(1):145-152.
[7] 吕超,刘丽萍,董慧茹,等.高效液相色谱-电感耦合等离子体质谱联用技术测定水产类膳食中5种砷形态的方法研究[J].分析测试学报,2010,29(5):465-468.
[8] 罗亚翠,冯舒凡,潘碧枢,等.加速溶剂萃取高效液相色谱-电感耦合等离子体质谱测定海产品中砷形态方法研究[J].中国卫生检验杂志,2017,33(14):2015-2019.
[9] 潘浩,李筱薇,宫智勇,等.高效液相色谱-电感耦合等离子体质谱法测定大米中无机砷方法研究[J].武汉工业学院学报,2012,31(3):1-5.
[10] 陈绍占,刘丽萍,杜宏举,等.高效液相色谱-电感耦合等离子体质谱法分析经牛黄解毒片暴露后大鼠血清中砷形态[J].质谱学报,2017,38(2):177-186.
[11] 黄北川,温良,李飞,等.LC-ICP-MS技术分析土壤中的砷形态[J].分析仪器,2018,23(1):43-48.
[12] 林琳,张素静,徐渭聪,等.血液和尿液中砷形态化合物的HPLC-ICP-MS分析[J].法医学杂志,2018,34(1):37-43.