Borsetti A P, Thurston L S
J Assoc Off Anal Chem. 1984 Mar-Apr;67(2):275-7.
A method is described for the determination of pentachlorophenol (PCP) in gelatin. The method employs acid and heat to hydrolyze the gelatin matrix, a base partition and wash for separation and cleanup, and a reacidification and extraction with hexane for direct determination of PCP, without preparation of a derivative, using gas chromatography (GC) with a 1% SP- 124ODA liquid phase and a 63Ni electron capture detector. Recoveries averaged 106% for fortifications between 0.02 and 1.0 ppm. The limit of quantitation is 20 ppb. The limit of detection is 4-6 ppb. The method, which has undergone a successful intralaboratory trial, is simple and rapid, and requires only general laboratory reagents and equipment. GC of the acetate derivative of PCP is used for confirmation of identity.
描述了一种测定明胶中五氯苯酚(PCP)的方法。该方法采用酸和热水解明胶基质,通过碱分配和洗涤进行分离与净化,再进行再酸化并用己烷萃取以直接测定PCP,无需制备衍生物,使用配备1% SP - 124ODA液相和63Ni电子捕获检测器的气相色谱(GC)。对于0.02至1.0 ppm的加标回收率平均为106%。定量限为20 ppb。检测限为4 - 6 ppb。该方法已成功通过实验室内部试验,简单快速,仅需一般实验室试剂和设备。PCP醋酸酯衍生物的GC用于确证。