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乳制品标准分析方法的精密度参数。

Precision parameters of standard methods of analysis for dairy products.

作者信息

Peeler J T, Horwitz W, Albert R

机构信息

Food and Drug Administration, Cincinnati, OH 45226.

出版信息

J Assoc Off Anal Chem. 1989 Sep-Oct;72(5):784-806.

PMID:2808241
Abstract

The available collaborative studies for standard methods of analysis for various constituents of milk and milk products were examined in an attempt to assign specific repeatability and reproducibility precision parameters to these methods. The different collaborative assays for the primary constituents (moisture/solids, fat, protein), the nutritionally important elements (calcium, sodium, potassium, phosphorus), and miscellaneous analytes/physical constants (ash, lactose, salt, freezing point) produced different estimates of the precision parameters for the same method. A suitable summary of the precision estimates from collaborative studies is given by the reproducibility relative standard deviation, RSDg, which is relatively constant within a product and permits comparisons across products. An estimate of the variation of RSDR for an analyte from a number of collaborative studies is presented in terms of the median and 90% interval (the range of the centermost 90% of values). These estimates are only informative when a substantial number of independent studies are available for pooling the independent estimates to form a distribution of RSDR values. The RSDR for the determination of the primary constituents of milk and milk products is characterized by a median RSDR of 1% and a 90% interval of 0.3-3%, with RSDR estimates occasionally occurring below 0.3% and above 4%. These overall estimates appear to be independent of analyte, matrix, and method and apply to concentrations of primary constituents that range from about 2 to 80%. The repeatability relative standard deviation, RSDr, is unstable, although it tends to converge to about 0.5-0.7 X RSDR. Too few collaborative assays are available to characterize RSDR for the determination of certain other constituents (acidity, ash, lactose, salt, and the nutritionally important elements) unless RSDR values for different analytes, methods, and matrixes are pooled on the basis of similar analyte concentrations. When pooled, the RSDR values are generally better than predicted from the Horwitz equation, RSDR (%) = 2 exp (1-0.5 log10C), where C is the concentration expressed as a decimal fraction; all but one of 661 RSDR values are within the upper empirical limit of twice this curve.

摘要

对现有的关于牛奶及奶制品各种成分标准分析方法的协作研究进行了审查,旨在为这些方法确定特定的重复性和再现性精密度参数。针对主要成分(水分/固形物、脂肪、蛋白质)、营养重要元素(钙、钠、钾、磷)以及其他分析物/物理常数(灰分、乳糖、盐分、冰点)的不同协作分析,对同一方法得出了不同的精密度参数估计值。协作研究精密度估计值的一个合适汇总由再现性相对标准偏差RSDg给出,它在一种产品内相对恒定,并且允许对不同产品进行比较。根据中位数和90%区间(值的最中间90%的范围)给出了来自多项协作研究的某分析物的RSDR变化估计值。只有当有大量独立研究可用于汇总独立估计值以形成RSDR值的分布时,这些估计值才具有参考价值。牛奶及奶制品主要成分测定的RSDR特征为,中位数RSDR为1%,90%区间为0.3 - 3%,RSDR估计值偶尔会低于0.3%或高于4%。这些总体估计值似乎与分析物、基质和方法无关,适用于含量范围约为2%至80%的主要成分。重复性相对标准偏差RSDr不稳定,尽管它往往会收敛到约0.5 - 0.7×RSDR。对于某些其他成分(酸度、灰分、乳糖、盐分以及营养重要元素)测定的RSDR,可用的协作分析太少,除非基于相似的分析物浓度汇总不同分析物、方法和基质的RSDR值。汇总后,RSDR值通常比根据霍维茨方程RSDR(%) = 2 exp(1 - 0.5 log10C)预测的要好,其中C是以小数表示的浓度;661个RSDR值中除一个之外,其他所有值都在该曲线两倍的经验上限之内。

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