Wei sheng yan jiu = Journal of hygiene research · 2010
[Mercury speciation in aquatic products analyzed by liquid chromatography cold vapor atomic fluorescence spectrometry].
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Shang Xiaohong, Zhao Yunfeng, Zhang Lei, Li Xiaowei, Wu Yongning
Аннотация
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.
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.