血清中多氯联苯测定的潜在分析方法评估：实验室间研究

Evaluation of potential analytical approach for determination of polychlorinated biphenyls in serum: interlaboratory study.

作者信息

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

出版信息

J Assoc Off Anal Chem. 1983 Jul;66(4):956-68.

Abstract

Forty-four laboratories participated in evaluation of a method for determining polychlorinated biphenyls (PCBs) as AR 1254 in serum at the parts per billion level. The method involves deproteinating serum with methanol, extracting with hexane-ethyl ether, and eluting PCBs from deactivated silica gel for gas-liquid chromatographic determination with electron capture detection. Compounds are quantitated by using the Webb-McCall factors. Five serum pools, 4 containing in vivo-fortified PCBs (as AR 1254) or 8 in vitro-fortified chlorinated hydrocarbons (CHs), or both, were used. For PCB fortification levels of 9.89 (EP 2), 24.74 (EP 3), and 74.20 ppb (EP 4), interlaboratory coefficients of variation (CVs) for collaborators that adhered to protocol were 92.7, 67.6, and 25.8%, respectively. CVs on the same pools analyzed by the Centers for Disease Control (CDC) were 7.4, 7.8, and 4.6%, respectively. Average interlaboratory recoveries for pools EP 2, EP 3, and EP 4 were 138.1, 111.2, and 91.1%, respectively, and 99.8, 89.6, and 90.4%, respectively, for CDC on the same pools. There was a general decrease in the mean error for those laboratories that had participated in an earlier study in which they were allowed to use their own methods.

摘要

44个实验室参与了一种用于测定血清中十亿分之一水平的多氯联苯（PCBs）（以AR 1254计）方法的评估。该方法包括用甲醇使血清脱蛋白，用己烷 - 乙醚萃取，以及从失活硅胶上洗脱多氯联苯以进行带电子捕获检测的气液色谱测定。通过使用Webb - McCall因子对化合物进行定量。使用了5个血清混合样本，其中4个含有体内强化的多氯联苯（以AR 1254计）或8种体外强化的氯代烃（CHs），或两者皆有。对于9.89（EP 2）、24.74（EP 3）和74.20 ppb（EP 4）的多氯联苯强化水平，遵循方案的协作实验室的实验室间变异系数（CVs）分别为92.7%、67.6%和25.8%。疾病控制中心（CDC）对相同混合样本进行分析得到的CVs分别为7.4%、7.8%和4.6%。EP 2、EP 3和EP 4混合样本的实验室间平均回收率分别为138.1%、111.2%和91.1%，而CDC对相同混合样本的回收率分别为99.8%、89.6%和90.4%。对于那些参与了早期研究（在该研究中允许他们使用自己的方法）的实验室，其平均误差普遍有所下降。