García-Rey R M, Quiles-Zafra R, de Castro M D Luque
Department of Analytical Chemistry, Marie Curie Building, Campus de Rabanales, University of Córdoba, 14071 Córdoba, Spain.
Anal Bioanal Chem. 2003 Sep;377(2):316-21. doi: 10.1007/s00216-003-2051-6. Epub 2003 Jul 19.
Focused microwave-assisted digestion and ultrasound leaching have been applied for the extraction of Pb, Cd, Cr, Cu, Fe, Zn, Ca, and Mg from raw meat. Semimembranous muscle (SM) of raw pig ham was used for optimizing both the digestion and extraction steps by multivariate approaches. The detection and quantification limits were 0.5 and 0.9 microg kg(-1) for Pb, 0.06 and 0.1 microg kg(-1) for Cd, 0.2 and 1.2 microg kg(-1) for Cr, 0.4 and 3 microg kg(-1) for Cu, 0.04 and 0.1 mg kg(-1) for Fe, 0.012 and 0.017 mg kg(-1) for Zn, 0.3 and 0.4 mg kg(-1) for Ca, and 0.01 and 0.03 mg kg(-1) for Mg. The precision, expressed as relative standard deviation (RSD), ranged between 2.5 and 9.6% for focused microwave-assisted digestion and between 3.5 and 10.6% for ultrasound leaching. The methods were then compared with a reference method and applied to a certified reference material (bovine muscle 184, from the BCR). The t-test, applied to the results obtained from focused microwave-assisted digestion, revealed that they are in agreement (p>0.01) with the certified and estimated values in the case of Pb, Cd, Cr, Cu, Fe, Ca, Mg, and Zn but not in that of Fe. In the case of ultrasound leaching, only the extraction of Pb, Cu, and Ca was quantitative. The method based on microwave digestion provides more accurate and precise results than ultrasound leaching. These new procedures have many advantages with regards to conventional methods, namely, reduction of the extraction time, simplification of the process, avoidance of chemical emissions to the atmosphere, and no losses of metals by volatilization.
聚焦微波辅助消解和超声浸提已应用于从生肉中提取铅、镉、铬、铜、铁、锌、钙和镁。生猪火腿的半膜肌(SM)被用于通过多变量方法优化消解和提取步骤。铅的检测限和定量限分别为0.5和0.9微克/千克,镉为0.06和0.1微克/千克,铬为0.2和1.2微克/千克,铜为0.4和3微克/千克,铁为0.04和0.1毫克/千克,锌为0.012和0.017毫克/千克,钙为0.3和0.4毫克/千克,镁为0.01和0.03毫克/千克。以相对标准偏差(RSD)表示的精密度,聚焦微波辅助消解在2.5%至9.6%之间,超声浸提在3.5%至10.6%之间。然后将这些方法与参考方法进行比较,并应用于有证标准物质(BCR的牛肌肉184)。对聚焦微波辅助消解获得的结果进行t检验表明,在铅、镉、铬、铜、铁、钙、镁和锌的情况下,它们与认证值和估计值一致(p>0.01),但铁的情况除外。在超声浸提的情况下,只有铅、铜和钙的提取是定量的。基于微波消解的方法比超声浸提提供更准确和精确的结果。这些新方法相对于传统方法有许多优点,即减少提取时间、简化过程、避免向大气排放化学物质以及无金属挥发损失。