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液相色谱-冷蒸气原子荧光光谱法分析水产品中的汞形态

[Mercury speciation in aquatic products analyzed by liquid chromatography cold vapor atomic fluorescence spectrometry].

作者信息

Shang Xiaohong, Zhao Yunfeng, Zhang Lei, Li Xiaowei, Wu Yongning

机构信息

Institute for Nutrition and Food Safety, China CDC, Beijing, 100021, China.

出版信息

Wei Sheng Yan Jiu. 2010 May;39(3):321-5.

Abstract

OBJECTIVE

To establish a method for the detection of mercury species in aquatic products by liquid chromatography online coupled with cold vapor atomic fluorescence spectrometry(LC-CV-AFS) and to participate in the international proficiency tests to verify the method.

METHODS

Mercury species were extracted from aquatic samples by using ultrasonication-assisted acid extraction, separated by reversed phase liquid chromatography, decomposed into inorganic mercury ion with on line UV digestion system, and then determined by cold vapor atomic fluorescence spectrometry.

RESULTS

Methylmercury, ethylmercury and inorganic mercury were baseline separated within 20 minutes. The linear range was 1-20 microg/L for the three species and the correlation coefficient r > or = 0.999. The detection limits for methylmercury, ethylmercury and inorganic mercury were 1 microg/kg, 2 microg/kg and 1 microg/kg respectively. The recovery of samples for three spiked levels (10, 50 and 500 microg/kg) was in the range of 89%-106%. The relative standard deviations (RSDs) were less than 10%. The determined methylmercury contents of certified reference materials (CRMs) were agreed well with the certified values. The results of determined methylmercury values were satisfied (Z <2) in two international proficiency tests, i.e., Food Analysis Performance Assessment Scheme (FAPAS, UK)-07115 test and International Atomic Energy Agency (IAEA)-452 test.

CONCLUSION

The LC-CV-AFS method is simple, sensitive and accurate and could meet the demand for mercury speciation in aquatic products.

摘要

目的

建立液相色谱在线联用冷蒸气原子荧光光谱法(LC-CV-AFS)检测水产品中汞形态的方法,并参加国际能力验证试验以验证该方法。

方法

采用超声辅助酸提取法从水产品样品中提取汞形态,经反相液相色谱分离,通过在线紫外消解系统将其分解为无机汞离子,然后用冷蒸气原子荧光光谱法测定。

结果

甲基汞、乙基汞和无机汞在20分钟内实现基线分离。三种汞形态的线性范围均为1 - 20μg/L,相关系数r≥0.999。甲基汞、乙基汞和无机汞的检出限分别为1μg/kg、2μg/kg和1μg/kg。三个加标水平(10、50和500μg/kg)的样品回收率在89% - 106%之间。相对标准偏差(RSDs)小于10%。有证标准物质(CRMs)中甲基汞的测定值与认定值吻合良好。在两项国际能力验证试验,即英国食品分析性能评估计划(FAPAS)-07115试验和国际原子能机构(IAEA)-452试验中,甲基汞测定结果均令人满意(Z<2)。

结论

LC-CV-AFS法简便、灵敏、准确,能够满足水产品中汞形态分析的需求。

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