Olalla Manuel, González Maria Cruz, Cabrera Carmen, Gimenez Rafael, López Maria Carmen
University of Granada, School of Pharmacy, Department of Nutrition and Bromatology, Spain.
J AOAC Int. 2002 Jul-Aug;85(4):960-6.
This paper describes a study of the different methods of sample preparation for the determination of calcium in grape juice, wines, and other alcoholic beverages by flame atomic absorption spectrometry; results are also reported for the practical application of these methods to the analysis of commercial samples produced in Spain. The methods tested included dealcoholization, dry mineralization, and wet mineralization with heating by using different acids and/or mixtures of acids. The sensitivity, detection limit, accuracy, precision, and selectiviy of each method were established. Such research is necessary because of the better analytical indexes obtained after acid digestion of the sample, as recommended by the European Union, which advocates the direct method. In addition, although high-temperature mineralization with an HNO3-HCIO4 mixture gave the best analytical results, mineralization with nitric acid at 80 degrees C for 15 min gave the most satisfactory results in all cases, including those for wines with high levels of sugar and beverages with high alcoholic content. The results for table wines subjected to the latter treatment had an accuracy of 98.70-99.90%, a relative standard deviation of 2.46%, a detection limit of 19.0 microg/L, and a determination limit of 31.7 microg/L. The method was found to be sufficiently sensitive and selective. It was applied to the determination of Ca in grape juice, different types of wines, and beverages with high alcoholic content, all of which are produced and widely consumed in Spain. The values obtained for Ca were 90.00 +/- 20.40 mg/L in the grape juices, 82.30 +/- 23.80 mg/L in the white wines, 85.00 +/- 30.25 mg/L in the sweet wines, 84.92 +/- 23.11 mg/L in the red wines, 85.75 +/- 27.65 mg/L in the rosé wines, 9.51 +/- 6.65 mg/L in the brandies, 11.53 +/- 6.55 mg/L in the gin, 7.3 +/- 6.32 mg/L in the pacharán, and 8.41 +/- 4.85 mg/L in the anisettes. The method is therefore useful for routine analysis in the quality control of these beverages.
本文描述了一项关于采用火焰原子吸收光谱法测定葡萄汁、葡萄酒及其他酒精饮料中钙含量时不同样品制备方法的研究;还报告了这些方法在分析西班牙生产的商业样品中的实际应用结果。所测试的方法包括脱醇、干法灰化以及使用不同酸和/或酸混合物加热的湿法灰化。确定了每种方法的灵敏度、检测限、准确度、精密度和选择性。由于按照欧盟的建议,样品经酸消解后能获得更好的分析指标,而欧盟提倡直接法,所以此类研究很有必要。此外,虽然用硝酸 - 高氯酸混合物进行高温灰化能得到最佳分析结果,但在所有情况下,包括对于高糖葡萄酒和高酒精度饮料,在80℃用硝酸灰化15分钟能得到最令人满意的结果。经后一种处理的佐餐葡萄酒的结果为:准确度98.70 - 99.90%,相对标准偏差2.46%,检测限19.0μg/L,测定限31.7μg/L。该方法被发现具有足够的灵敏度和选择性。它被应用于测定葡萄汁、不同类型葡萄酒以及高酒精度饮料中的钙含量,所有这些产品均在西班牙生产且广泛消费。葡萄汁中钙的测定值为90.00±20.40mg/L,白葡萄酒中为82.30±23.80mg/L,甜葡萄酒中为85.00±30.25mg/L,红葡萄酒中为84.92±23.11mg/L,桃红葡萄酒中为85.75±27.65mg/L,白兰地中为9.51±6.65mg/L,杜松子酒中为11.53±6.55mg/L,帕查兰酒中为7.3±6.32mg/L,茴芹酒中为8.41±4.85mg/L。因此,该方法对于这些饮料质量控制中的常规分析很有用。