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低温消解后采用常规高灵敏度冷蒸气原子吸收光谱法测定食品中的总汞。

Routine, high-sensitivity, cold vapor atomic absorption spectrometric determination of total mercury in foods after low-temperature digestion.

作者信息

Dabeka Robert W, Bradley Peter, McKenzie Arthur D

机构信息

Health Canada, Health Products and Food Branch, Food Research Division, Ottawa, ON.

出版信息

J AOAC Int. 2002 Sep-Oct;85(5):1136-43.

PMID:12374414
Abstract

A cold vapor atomic absorption spectrometric method was developed for the subnanogram-per-gram determination of total Hg in a wide variety of foods. Foods were weighed into 50 mL polypropylene centrifuge tubes and dried without charring at 55 degrees C in a circulating oven. Samples were then digested at 58 degrees C with HNO3, HCl, and H2O2. After matrix modification with solutions of 2% Mg(NO3)2, 0.01% Triton X-100, and Cu(II) at 10 microg/mL, samples were analyzed by using a CeTAC Technologies M-6000A dedicated Hg analyzer. Based on a 2 g sample weight, the detection limit of the method over 12 batches averaged 0.30 ng/g wet weight and ranged from 0.03 to 0.6 ng/g. Recoveries of Hg added to 17 different foods, analyzed in a routine manner, averaged 97%, and individual recoveries ranged from 77 to 107%. Accuracy was confirmed by analysis of 7 biological reference materials from the National Research Council of Canada and the National Institute of Standards and Technology. Stabilization of low concentrations of Hg in solutions containing no sample was required to prevent loss of Hg from blanks. In a comparison of NaCl, potassium dichromate, and Au(II), chloride was much more effective for stabilization than the other two, and HCl was used for subsequent stabilization.

摘要

建立了一种冷蒸气原子吸收光谱法,用于测定各种食品中低至纳克每克水平的总汞含量。将食品称入50 mL聚丙烯离心管中,在循环烘箱中于55℃干燥而不碳化。然后样品在58℃下用硝酸、盐酸和过氧化氢进行消解。在用2%硝酸镁、0.01% Triton X - 100和10μg/mL的铜(II)溶液进行基体改进后,使用CeTAC Technologies M - 6000A专用汞分析仪对样品进行分析。基于2 g的样品重量,该方法在12批次分析中的检测限平均为0.30 ng/g湿重,范围为0.03至0.6 ng/g。以常规方式分析添加到17种不同食品中的汞,回收率平均为97%,个别回收率范围为77%至107%。通过分析加拿大国家研究委员会和美国国家标准与技术研究院的7种生物参考物质来确认准确性。为防止空白样品中汞的损失,需要对不含样品的溶液中的低浓度汞进行稳定化处理。在比较氯化钠、重铬酸钾和金(II)时,氯化物在稳定化方面比其他两种更有效,随后使用盐酸进行稳定化处理。

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