微波辅助-液相色谱-原子荧光光谱法对水产品中汞的形态分析  

Morphological analysis of mercury in aquatic products by mirowave assisted-liquid chromatography-atomic fluorescence spectrometry

作　　者：王媛[1] 张宏斌[1] 陆巧荣[1] 孙成均[2] 

机构地区：[1]昆山市疾病预防控制中心,江苏昆山215300 [2]四川大学华西医学中心,四川成都610041

出　　处：《中国卫生检验杂志》2016年第21期3101-3104,共4页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立微波辅助-液相色谱-原子荧光光谱联用分析方法(HPLC-AFS)测定水产品中的无机汞、甲基汞、乙基汞、二苯基汞,并且研究了水产品的样品前处理方法。方法样品经提取液6 mol/L盐酸+0.10 mol/L氯化钠+0.2%L-半胱氨酸5 ml微波萃取后,调节p H值,提取液净化后,注入HPLC-AFS分析。结果无机汞、甲基汞、乙基汞的浓度为0.5μg/L^100μg/L时,线性关系良好,相关系数(r)均为0.999 9,检出限分别为2.08μg/kg、1.41μg/kg、1.36μg/kg。二苯基汞在盐酸介质中发生了分解。方法的日内精密度为3.65%,日间精密度为5.14%。采用BCR-463金枪鱼、GBW10024扇贝、GBW08573黄鱼标准物质对测定方法的准确度进行验证,结果都在给定的参考值范围内。结论本方法操作简便、快速、灵敏、准确,可满足鲜活水产中无机汞、甲基汞、乙基汞的测定,不适用样品中二苯基汞的提取检测。Objective To establish a method for the determination of methyl-,ethyl-,diphenyl-,inorganic mercury in aquatic products by liquid chromatography- atomic fluorescence spectrometry（ LC- AFS）. And the pretreatment methods of aquatic products sample were studied. Methods The samples were extracted with 5 ml extractant solution containing 6 mol / L HCl with 0. 10 mol / L Na Cl and 0. 2% L- cysteine by microwave,adjusting p H. The extractant solution was cleaned and then injected into the HPLC- AFS system for analysis. Results Good linearity was obtained when the concentrations of methyl-,ethyl-,inorganic mercury were within 0. 5 μg / L- 100 μg / L,and the correlation coefficient（ r） was 0. 999 9,with the detection limits of 2. 08 μg / kg,1. 41 μg / kg,1. 36 μg / kg,respectively. Diphenylmercury was found to be partially decomposed when it was in the medium of hydrogen chloride. The within- day precision of the method was 3. 65% and between- day precision was 5. 14%. Certified reference materials（ BCR- 463 tuna,GBW10024 scallop and GBW08573 yellow- fin tuna） were used to validate the accuracy of this new established method,and the measured values were all accommodated with the given values. Conclusion The proposed method was simple,rapid,sensitive and accurate,and suitable for the detection of methyl-,ethyl-,inorganic mercury in aquatic products,but not suitable for the detection of diphenylmercury.

关 键 词：水产品 甲基汞 形态分析 液相色谱-原子荧光光谱法 微波辅助 

分 类 号：O657.31[理学—分析化学]