Heikes D L, Griffitt K R
J Assoc Off Anal Chem. 1980 Sep;63(5):1125-7.
A method was developed for the determination of pentachlorophenol (PCP) in the seals and enamel of Mason lids. After extraction with acidic CH2Cl2 and methylation, the resulting pentachloroanisole was determined by gas-liquid chromatography (GLC) with electron capture detection (EC). Three of the 9 brands of lids examined contained PCP. Levels were as high as 198 micrograms/lid. Recoverires from fortified samples ranged from 92 to 103%. Six fruits and vegetables were canned by home canning techniques, using lids shown to contain PCP. PCP in these foods was determined by a procedure specifying extraction with acidic CH2Cl2 and gel permeation chromatography cleanup. Extracts were methylated and determined by GLC-EC. PCP was found in all the canned foods. Levels were as high as 16 micrograms/qt. Recoveries from foods fortified with PCP ranged from 85 to 94%. The presence of PCP was confirmed by GLC-mass spectrometric determination of the derivative, pentachloroanisole.
开发了一种测定梅森瓶盖密封垫和珐琅中五氯苯酚(PCP)的方法。用酸性二氯甲烷萃取并甲基化后,通过带有电子捕获检测(EC)的气液色谱法(GLC)测定生成的五氯苯甲醚。所检测的9个品牌瓶盖中有3个含有五氯苯酚。含量高达198微克/个瓶盖。加标样品的回收率在92%至103%之间。使用显示含有五氯苯酚的瓶盖,通过家庭罐装技术对6种水果和蔬菜进行罐装。这些食品中的五氯苯酚通过规定用酸性二氯甲烷萃取和凝胶渗透色谱净化的程序进行测定。提取物经甲基化后用GLC-EC测定。在所有罐装食品中均发现了五氯苯酚。含量高达16微克/夸脱。五氯苯酚加标食品的回收率在85%至94%之间。通过对衍生物五氯苯甲醚进行GLC-质谱测定,证实了五氯苯酚的存在。