吹扫捕集-气相色谱-原子荧光光谱法测定水产饲料中的甲基汞
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摘要
称取约0.2g水产饲料样品,加入250g·L~(-1)氢氧化钾-甲醇溶液10mL,于60℃加热6h,每隔2h涡旋振荡一次,然后以3 000r·min~(-1)转速离心15min,取0.10mL上清液加入提前加入34～38mL水的40 mL棕色进样瓶内,用盐酸(1+9)溶液调节pH至6～8后,再加入2mol·L~(-1)乙酸钠缓冲溶液0.3 mL和乙基化试剂0.05 mL,进行衍生化反应后,加水定容至40.0mL,混匀后用吹扫捕集-气相色谱-原子荧光光谱仪进行测定。结果表明:甲基汞的质量在500pg内与荧光强度呈线性关系,方法的检出限(3s/k)为2μg·kg~(-1),测定下限(10s/k)为5μg·kg~(-1)。加标回收率在94.7%～98.8%之间,测定值的相对标准偏差(n=6)为4.9%。
The aquatic feed sample(about 0.2 g) was added into 10 mL of 250 g·L~(-1) potassium hydroxidemethanol solution.The mixture was heated at 60 ℃ for 6 h,vortex oscillated every 2 h,then centrifuged at 3 000 r·min~(-1) for 15 min.0.10 mL of the supernatant was added into a 40 mL brown sample bottle with 34-38 mL of water added in advance,and the pH of the solution was adjusted to 6-8 with HCl(1+9) solution.0.3 mL of 2 mol·L~(-1) sodium acetate buffer solution and 0.05 mL of ethylation reagent were added to carry out derivatization.Then the solution was made up to 40.0 mL with water.After mixing well,purge and trap-gas chromatography-atomic fluorescence spectrometer was used for determination.The results showed that the fluorescence intensity was kept linear with the mass of methylmercury within 500 pg.The detection limit(3 s/k) of the method was 2μg·kg~(-1),and the lower limit of determination(10 s/k) was 5μg·kg~(-1).Values of recovery obtained by standard addition method were between 94.7% and 98.8%,and the relative standard deviation(n=6) of determined values was 4.9%.
The aquatic feed sample(about 0.2 g) was added into 10 mL of 250 g·L~(-1) potassium hydroxidemethanol solution.The mixture was heated at 60 ℃ for 6 h,vortex oscillated every 2 h,then centrifuged at 3 000 r·min~(-1) for 15 min.0.10 mL of the supernatant was added into a 40 mL brown sample bottle with 34-38 mL of water added in advance,and the pH of the solution was adjusted to 6-8 with HCl(1+9) solution.0.3 mL of 2 mol·L~(-1) sodium acetate buffer solution and 0.05 mL of ethylation reagent were added to carry out derivatization.Then the solution was made up to 40.0 mL with water.After mixing well,purge and trap-gas chromatography-atomic fluorescence spectrometer was used for determination.The results showed that the fluorescence intensity was kept linear with the mass of methylmercury within 500 pg.The detection limit(3 s/k) of the method was 2μg·kg~(-1),and the lower limit of determination(10 s/k) was 5μg·kg~(-1).Values of recovery obtained by standard addition method were between 94.7% and 98.8%,and the relative standard deviation(n=6) of determined values was 4.9%.
引文
[1] 戴礼洪,刘潇威,王迪,等.固相萃取-高效液相色谱-原子荧光光谱法联用测定水中无机汞(Ⅱ)及有机汞[J].理化检验-化学分册,2015,51(8):1178-1182.
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[9] 陈德泉,李岩,叶泽波.加速溶剂提取-液相色谱-原子荧光光谱法测定对虾饲料中5种形态的汞[J].理化检验-化学分册,2018,54(6):698-702.
[10] 傅雄伟,李海普,杨远,等.高效液相色谱与电感耦合等离子体质谱联用测定水中的二价汞、甲基汞与乙基汞[J].理化检验-化学分册,2016,52(11):1277-1281.
[11] 欧阳珮珮,黄诚,丘福保.高效液相色谱-电感耦合等离子体质谱法同时测定水产品中的无机汞、甲基汞和乙基汞[J].中国卫生检验杂志,2016,26(1):50-53.
[12] 崔颖,肖亚兵,王禹,等.P&T-GC-CVAFS法测定海产动物中的甲基汞和乙基汞[J].食品研究与开发,2016,37(1):145-148.
[13] 顾昱晓,孟梅,邵俊娟,等.在线吹扫捕集-气相色谱-原子荧光光谱法测定土壤中甲基汞[J].分析化学,2013,41(11):1754-1757.
[14] 陈来国,田文娟,莫测辉,等.全自动甲基汞分析系统分析甲基汞的仪器条件优化[J].环境化学,2011,30(7):1332-1336.
[15] MARCINKOWSKA M,BARALKIEWICZ D.Multielemental speciation analysis by advanced hyphenated technique-HPLC/ICP-MS:A review[J].Talanta,2016,161(12):177-204.
[2] EKINL S,SUSA M,NINOMIYA T,et al.Mijamata disease revisted:An update on the acute and chronic manifestations of methylmercury poisoning[J].Journal of the Neurological Sciences,2007,262(1):131-144.
[3] 梅光明,张小军,钟志,等.浙江沿海海产品甲基汞污染调查及膳食风险评估[J].食品科学,2016,37(17):207-212.
[4] LI P,FENG X B,YUAN X B,et al.Rice consumption contributes to low methylmercury exposure in southern China[J].Environment International,2012,49(1):18-23.
[5] ZHANG L,WONG M H.Environmental methylmercury contamination in China:Sources and impacts[J].Environment International,2007,33(1):108-121.
[6] 温权,苏祖俭,蔡文华,等.食品中甲基汞检测技术研究进展[J].食品安全质量检测学报,2017,8(3):845-853.
[7] 武晓燕,古晓娜,马跃峰,等.土壤中甲基汞含量水平及分析方法概述[J].环境与职业医学,2015,32(11):1078-1083.
[8] 曾云想,梁婷婷,汤明河,等.液相色谱-原子荧光光谱法测定水产品中汞形态的含量[J].理化检验-化学分册,2017,53(10):1226-1228.
[9] 陈德泉,李岩,叶泽波.加速溶剂提取-液相色谱-原子荧光光谱法测定对虾饲料中5种形态的汞[J].理化检验-化学分册,2018,54(6):698-702.
[10] 傅雄伟,李海普,杨远,等.高效液相色谱与电感耦合等离子体质谱联用测定水中的二价汞、甲基汞与乙基汞[J].理化检验-化学分册,2016,52(11):1277-1281.
[11] 欧阳珮珮,黄诚,丘福保.高效液相色谱-电感耦合等离子体质谱法同时测定水产品中的无机汞、甲基汞和乙基汞[J].中国卫生检验杂志,2016,26(1):50-53.
[12] 崔颖,肖亚兵,王禹,等.P&T-GC-CVAFS法测定海产动物中的甲基汞和乙基汞[J].食品研究与开发,2016,37(1):145-148.
[13] 顾昱晓,孟梅,邵俊娟,等.在线吹扫捕集-气相色谱-原子荧光光谱法测定土壤中甲基汞[J].分析化学,2013,41(11):1754-1757.
[14] 陈来国,田文娟,莫测辉,等.全自动甲基汞分析系统分析甲基汞的仪器条件优化[J].环境化学,2011,30(7):1332-1336.
[15] MARCINKOWSKA M,BARALKIEWICZ D.Multielemental speciation analysis by advanced hyphenated technique-HPLC/ICP-MS:A review[J].Talanta,2016,161(12):177-204.