淡水鱼中无机砷的液相色谱-原子荧光光谱测定法
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摘要
目的建立液相色谱-原子荧光光谱法测定淡水鱼中无机砷[AS(Ⅲ),AS(Ⅴ)]的方法。方法准确称取鱼肉1.0 g,用0.15 mol/L硝酸于60℃超声提取40 min,加正己烷除去杂质后经0.45μm有机滤膜过滤及C18小柱净化。采用Hamilton PRP X-100阴离子交换柱(150 mm×4.1 mm,10μm)分离,磷酸氢二钠和磷酸二氢钾(pH=4.0)为流动相等梯度洗脱,流速1.3 ml/min,用原子荧光检测。保留时间定性,外标法定量。结果 2种砷形态线性关系良好(r>0.999),方法检出限AS(Ⅲ)为0.017 mg/kg,AS(Ⅴ)为0.050 mg/kg。平均回收率为85.4%～103.8%,精密度为1.1%～3.4%。结论本方法操作简便、结果准确、精密度高,适用于同时检测淡水鱼中2种形态的无机砷AS(Ⅲ)和AS(Ⅴ)。
[Objective]To establish a method for the determination of inorganic arsenic [AS(Ⅲ),AS(Ⅴ)] in freshwater fish by liquid chromatography-atomic fluorescence spectrometry.[Methods]1.0 g of fish meat was accurately weighed and extracted with0.15 mol/L nitric acid at 60 ℃ for 40 min. After adding hexane,the mixture was filtered through 0.45μm organic membrane and purified by C18 cartridge,then separated by Hamilton PRP X-100 anion exchange column(150 mm ×4.1 mm,10 μm). The disodium hydrogen phosphate and potassium dihydrogen phosphate(pH=4.0) were used as mobile phase in flow-equal gradient elution at a flow rate of 1.3 ml/min,and atomic fluorescence detection was performed. The retention time was used for qualitative detection and external standard method was used for quantification.[Results]The linear relationships of the two arsenic species were good(r>0.999). The detection limit of AS(Ⅲ) and AS(Ⅴ) was 0.017 mg/kg and 0.050 mg/kg respectively.The average recovery was85.4%-103.8%,and the precision was 1.1%-3.4%.[Conclusion]This method is simple and accurate,with high precision. It is suitable for simultaneous detection of two forms of inorganic arsenic AS(Ⅲ) and AS(Ⅴ) in freshwater fish.
[Objective]To establish a method for the determination of inorganic arsenic [AS(Ⅲ),AS(Ⅴ)] in freshwater fish by liquid chromatography-atomic fluorescence spectrometry.[Methods]1.0 g of fish meat was accurately weighed and extracted with0.15 mol/L nitric acid at 60 ℃ for 40 min. After adding hexane,the mixture was filtered through 0.45μm organic membrane and purified by C18 cartridge,then separated by Hamilton PRP X-100 anion exchange column(150 mm ×4.1 mm,10 μm). The disodium hydrogen phosphate and potassium dihydrogen phosphate(pH=4.0) were used as mobile phase in flow-equal gradient elution at a flow rate of 1.3 ml/min,and atomic fluorescence detection was performed. The retention time was used for qualitative detection and external standard method was used for quantification.[Results]The linear relationships of the two arsenic species were good(r>0.999). The detection limit of AS(Ⅲ) and AS(Ⅴ) was 0.017 mg/kg and 0.050 mg/kg respectively.The average recovery was85.4%-103.8%,and the precision was 1.1%-3.4%.[Conclusion]This method is simple and accurate,with high precision. It is suitable for simultaneous detection of two forms of inorganic arsenic AS(Ⅲ) and AS(Ⅴ) in freshwater fish.
引文
[1]林燕奎,王丙涛,颜治,等.食用菌中的总砷和砷形态分布研究[J].食品科技,2012,37(5):295-299.
[2]王继霞,胡蔚娜,叶明德,等.贝壳类海产品砷形态分析实验研究[J].实验室技术与管理,2016,33(10):45-48,54.
[3]陈竞秀.液相-原子荧光法测定食品中无机砷[J].广东化学,2018,45(20):140-145.
[4]王婧,党献文,潘静,等.液相色谱-原子荧光光谱法测定大米中无机砷[J].粮食与饲料工业,2017(2):61-64.
[5]陈红红,毋福海,黄丽玫,等.广州市场食用鱼中5种重金属含量分析及评价[J].中国卫生检验杂志,2008,18(12):2736-2738.
[6]曹立,郭小娟.慢性砷暴露与砷毒性的研究新进展[J].医学综述,2014,20(17):3161-3163.
[7]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5种砷形态[J].色谱,2014,32(7):717-722.
[8]净锦飞,徐焰,骆文静,等.亚慢性砷暴露对大鼠肾脏功能和形态的影响[J].实用预防医学,2011,18(2):195-198.
[9]张华,王英锋,施燕支,等.高效液相色谱及联用技术在砷形态分析中的应用[J].光谱学与光谱分析,2007,27(2):389-390.
[10]李娜,郑国华,罗海恩,等.液相色谱-原子荧光光谱法测定海参中的无机砷[J].广州化学,2018,43(3):44-46.
[11]胡容,张颖,徐全金,等.液相色谱-原子荧光联用法测定大米中的无机砷含量[J].贵州科学,2017,35(1):87-89.
[12]刘芸,王小平.液相色谱-原子荧光光谱法无机砷测定的探讨[J].粮食储藏,2018,47(4):53-56.
[13]胥佳佳,冯鑫,汤静,等.超声辅助提取-高效液相色谱-电感耦合等离子体质谱法测定香菇中6种形态砷化合物[J].食品科学,2016,37(24):216-221.
[14]李晓玉,刘丽萍,陈绍占.高效液相色谱-电感耦合等离子体质谱法测定保健品食品类袋泡茶中5种砷形态[J].中国食品卫生杂志,2018,30(5):491-496.
[15]刘峰,石志芳,姜霞,等.HPLC-ICP-MS法分析太湖沉积物中砷的形态及分布特征[J].质谱学报,2011,32(3):170-175.
[16]陆奕娜,陈建伟,张林田,等.高效液相色谱-电感耦合等离子体质谱同时测定虾类中6种砷形态[J].分析科学学报,2016,32(1):141-144.
[17]祖文川,汪雨,刘聪,等.高效液相色谱-原子荧光光谱联用技术分析6种植物源性中药中砷的形态[J].分析试验室,2016,35(1):82-85.
[18]苏祖俭,黄伟雄,蔡文华,等.食品中无机砷分析技术进展[J].食品安全质量检测学报,2018,9(14):3580-3589.
[2]王继霞,胡蔚娜,叶明德,等.贝壳类海产品砷形态分析实验研究[J].实验室技术与管理,2016,33(10):45-48,54.
[3]陈竞秀.液相-原子荧光法测定食品中无机砷[J].广东化学,2018,45(20):140-145.
[4]王婧,党献文,潘静,等.液相色谱-原子荧光光谱法测定大米中无机砷[J].粮食与饲料工业,2017(2):61-64.
[5]陈红红,毋福海,黄丽玫,等.广州市场食用鱼中5种重金属含量分析及评价[J].中国卫生检验杂志,2008,18(12):2736-2738.
[6]曹立,郭小娟.慢性砷暴露与砷毒性的研究新进展[J].医学综述,2014,20(17):3161-3163.
[7]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5种砷形态[J].色谱,2014,32(7):717-722.
[8]净锦飞,徐焰,骆文静,等.亚慢性砷暴露对大鼠肾脏功能和形态的影响[J].实用预防医学,2011,18(2):195-198.
[9]张华,王英锋,施燕支,等.高效液相色谱及联用技术在砷形态分析中的应用[J].光谱学与光谱分析,2007,27(2):389-390.
[10]李娜,郑国华,罗海恩,等.液相色谱-原子荧光光谱法测定海参中的无机砷[J].广州化学,2018,43(3):44-46.
[11]胡容,张颖,徐全金,等.液相色谱-原子荧光联用法测定大米中的无机砷含量[J].贵州科学,2017,35(1):87-89.
[12]刘芸,王小平.液相色谱-原子荧光光谱法无机砷测定的探讨[J].粮食储藏,2018,47(4):53-56.
[13]胥佳佳,冯鑫,汤静,等.超声辅助提取-高效液相色谱-电感耦合等离子体质谱法测定香菇中6种形态砷化合物[J].食品科学,2016,37(24):216-221.
[14]李晓玉,刘丽萍,陈绍占.高效液相色谱-电感耦合等离子体质谱法测定保健品食品类袋泡茶中5种砷形态[J].中国食品卫生杂志,2018,30(5):491-496.
[15]刘峰,石志芳,姜霞,等.HPLC-ICP-MS法分析太湖沉积物中砷的形态及分布特征[J].质谱学报,2011,32(3):170-175.
[16]陆奕娜,陈建伟,张林田,等.高效液相色谱-电感耦合等离子体质谱同时测定虾类中6种砷形态[J].分析科学学报,2016,32(1):141-144.
[17]祖文川,汪雨,刘聪,等.高效液相色谱-原子荧光光谱联用技术分析6种植物源性中药中砷的形态[J].分析试验室,2016,35(1):82-85.
[18]苏祖俭,黄伟雄,蔡文华,等.食品中无机砷分析技术进展[J].食品安全质量检测学报,2018,9(14):3580-3589.
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