Pollman R M
New York State Food Laboratory, Department of Agriculture and Markets, Albany 12235.
J Assoc Off Anal Chem. 1991 Jan-Feb;74(1):27-31.
The determination of calcium, phosphorus, and magnesium in cheese was collaboratively studied. The sample is dried and ashed and the residue is dissolved in an acidified aqueous solution. Calcium and magnesium are determined by atomic absorption spectrophotometry and phosphorus is determined by colorimetry. The study was repeated 3 times because of high within- and between-laboratory relative standard deviations (RSDr and RSDR, respectively). Poor precision in the first 2 studies was caused by a number of factors, including use of contaminated glassware, improperly maintained instruments, and impure reagents as standards. In each study, 5 varieties of cheese were distributed as 10 blind duplicate samples along with a practice sample. Thirteen laboratories participated in the third study, which was generally problem-free. The range of results and the average RSDr and RSDR found in the cheeses were: calcium, 608-1107 mg/100 g. 1.5%, 2.6%; magnesium, 23.9-50.6 mg/100 g, 2.8%, 3.8%; phosphorus, 444-695 mg/100 g, 1.2%, 1.6%. The method has been adopted official first action by AOAC.
对奶酪中的钙、磷和镁含量测定进行了协同研究。将样品干燥并灰化,残留物溶解于酸化水溶液中。钙和镁采用原子吸收分光光度法测定,磷采用比色法测定。由于实验室内和实验室间的相对标准偏差(分别为RSDr和RSDR)较高,该研究重复进行了3次。前两项研究中精密度较差是由多种因素导致的,包括使用受污染的玻璃器皿、仪器维护不当以及作为标准品的试剂不纯。在每项研究中,将5种奶酪作为10个盲样重复样品以及1个练习样品进行分发。13个实验室参与了第三次研究,该次研究总体上没有问题。奶酪中得到的结果范围以及平均RSDr和RSDR分别为:钙,608 - 1107 mg/100 g,1.5%,2.6%;镁,23.9 - 50.6 mg/100 g,2.8%,3.8%;磷,444 - 695 mg/100 g,1.2%,1.6%。该方法已被AOAC采用为首次官方方法。