血清中多氯联苯（以氯丹1254计）的气相色谱测定：协作研究

Gas chromatographic determination of polychlorinated biphenyls (as Aroclor 1254) in serum: collaborative study.

作者信息

Burse V W, Korver M P, Needham L L, Lapeza C R, Boozer E L, Head S L, Liddle J A, Bayse D D

机构信息

Division of Environmental Health Laboratory Sciences, Atlanta, GA 30333.

出版信息

J Assoc Off Anal Chem. 1989 Jul-Aug;72(4):649-59.

PMID:2547752

Abstract

A gas chromatographic-electron capture detection method for determining the concentration of polychlorinated biphenyls (PCBs) as Aroclor 1254 (AR 1254) in serum was evaluated through a 2-phase collaborative study. In Phase I, each collaborator's lot of Woelm silica gel (70-150 mesh) was evaluated for elution and recovery of AR 1254, which had been added in vitro at 25 ng/mL to a serum extract. In Phase II, each collaborator analyzed a series of bovine serum samples that contained the following: (1) in vitro-spiked AR 1254; (2) in vivo AR 1254 and 8 in vitro-spiked chlorinated hydrocarbons; (3) in vivo AR 1254 only; (4) 8 in vitro-spiked chlorinated hydrocarbons only; and (5) neither AR 1254 nor chlorinated hydrocarbons above the detection limit of the method. In Phase I, the average recovery of AR 1254 from silica gel for the 6 collaborators was 87.9 +/- 15.44% (mean +/- 1 SD; N = 18; range = 52.3-105.8%). In Phase II, the analysis of in vitro spikes of AR 1254 in serum at 8.58, 16.8, 41.8, and 84.3 ppb gave mean (means) interlaboratory recoveries of 89.0, 83.3, 79.4, and 76.9%, respectively, with within-laboratory (repeatability) relative standard deviations (RSDr) of 18.8, 20.5, 10.2, and 14.1%, respectively, and among-laboratory (reproducibility) relative standard deviations (RSDR) of 21.5, 21.1, 14.6, and 20.8%, respectively. The determination of in vivo AR 1254 in samples containing approximately 10, 25, 50, and 100 ng/mL of AR 1254 resulted in interlaboratory means of 10, 22, 39, and 79 ng/mL, respectively, with RSDr = 6.7, 9.7, 6.4, and 5.8%, respectively, and RSDR = 20.6, 16.0, 10.9, and 10.3%, respectively. The precision of the method for incurred AR 1254 showed a maximum RSDr of less than 10% and a maximum RSDR of less than 21% for a concentration range of 10-100 ng/mL. The accuracy of the method as demonstrated by the mean recovery of in vitro-spiked AR 1254 over a concentration range of 8.58-843 ng/mL was 82.2%. The method has been approved interim official first action.

摘要

通过一项两阶段合作研究，对一种用于测定血清中多氯联苯（PCBs）以Aroclor 1254（AR 1254）形式存在的浓度的气相色谱 - 电子捕获检测方法进行了评估。在第一阶段，对每位合作者的沃姆硅胶（70 - 150目）批次进行评估，以检测其对在体外以25 ng/mL添加到血清提取物中的AR 1254的洗脱和回收率。在第二阶段，每位合作者分析了一系列牛血清样本，这些样本包含以下几种情况：（1）体外添加AR 1254的样本；（2）体内含有AR 1254和8种体外添加的氯代烃的样本；（3）仅体内含有AR 1254的样本；（4）仅含有8种体外添加的氯代烃的样本；以及（5）既不含有AR 1254也不含有高于该方法检测限的氯代烃的样本。在第一阶段，6位合作者从硅胶中回收AR 1254的平均回收率为87.9 +/- 15.44%（平均值 +/- 1标准差；N = 18；范围 = 52.3 - 105.8%）。在第二阶段，对血清中浓度为8.58、16.8、41.8和84.3 ppb的体外添加AR 1254进行分析，实验室间平均回收率分别为89.0%、83.3%、79.4%和76.9%，实验室内（重复性）相对标准偏差（RSDr）分别为18.8%、20.5%、10.2%和14.1%，实验室间（再现性）相对标准偏差（RSDR）分别为21.5%、21.1%、14.6%和20.8%。对含有大约10、25、50和100 ng/mL AR 1254的样本中体内AR 1254的测定，实验室间平均值分别为10、22、39和79 ng/mL，RSDr分别为6.7%、9.7%、6.4%和5.8%，RSDR分别为20.6%、16.0%、10.9%和10.3%。该方法对实际存在的AR 1254的精密度在浓度范围为10 - 100 ng/mL时，最大RSDr小于10%，最大RSDR小于21%。在8.58 - 843 ng/mL浓度范围内，体外添加AR 1254的平均回收率所证明的该方法的准确度为82.2%。该方法已被批准为暂行官方首次行动方法。