Veierov D, Aharonson N
J Assoc Off Anal Chem. 1978 Mar;61(2):253-60.
A new cleanup procedure is described for chlorinated hydrocarbon residues in butterfat. The method is based on the dropwise addition of H2SO4 to a fat solution column and continuous removal of the lipids and the acid. The cleanup of 0.25-2.0 g fat requires only 10-40 ml sulfuric acid and 12-17 ml petroleum ether. There is no need for any further cleanup step, solvent evaporation, or centrifugation. The method is easy to standardize and is suitable for automation. At least 30 fat samples can be cleaned up manually by one analyst in one day. Recoveries were complete (greater than 90%) for polychlorinated biphenyl compounds and for 13 chlorinated pesticides of 16 examined. The method was tested on chlorinated hydrocarbon residues in commercial butter and the results were compared with those obtained with the acetonitrile method. The versatility and limitations of the method were investigated by varying the sulfuric acid strength, initial fat solution concentration, and column dimensions.
本文描述了一种用于清除乳脂肪中氯代烃残留的新净化程序。该方法基于向脂肪溶液柱中逐滴加入硫酸，并持续去除脂质和酸。净化0.25 - 2.0克脂肪仅需10 - 40毫升硫酸和12 - 17毫升石油醚。无需任何进一步的净化步骤、溶剂蒸发或离心操作。该方法易于标准化且适合自动化。一名分析人员一天内可手动净化至少30个脂肪样品。对于多氯联苯化合物以及所检测的16种氯代农药中的13种，回收率均达到完全（大于90%）。该方法在市售黄油中的氯代烃残留检测中进行了测试，并将结果与乙腈法所得结果进行了比较。通过改变硫酸强度、初始脂肪溶液浓度和柱尺寸，研究了该方法的通用性和局限性。
