Hao Lili, Xue Jian
Institute of Medicinal Plant Development, Chinese Academy of Medical Science and Peking Union Medical College, Beijing 100094, China.
J Chromatogr Sci. 2006 Sep;44(8):518-22. doi: 10.1093/chromsci/44.8.518.
A simple and efficient method for simultaneous gas chromatographic (GC) determination of 18 organochlorine pesticides [tecnazene, hexachlorobenzene, alpha-benzenehexachloride (BHC), pentachloronitrobenzene (PCNB), gamma-BHC, heptachlor, aldrin, methyl pentachlorophenyl sulfide, beta-BHC, delta-BHC, heptachlor epoxide, alpha-endosulfan, trans-chlorodane, cis-chlorodane, p,p'-dichlorodiphenyl dichloroethylene, o,p'-DDT, p,p'-DDD, and p,p'-DDT] in Traditional Chinese Medicine (TCM) is described. The procedure involves ultrasonic extraction and sulphuric acid treatment as the cleanup method. Detection of the sample is performed by GC-electron capture detection. A series of experiments are conducted to optimize the final pretreatment conditions [acetone-petroleum ether (1:1) as the extract solvent, ultrasonication for 15 min, three steps, concentrated sulphuric acid with 10% water for sulphuric acid treatment]. Recovery studies are performed at 10, 50, and 100 parts-per-billion (ppb) fortification levels of each organochlorine pesticide, except for alpha-endosulfan, which are 20, 100, and 200 ppb. The percentage recoveries range from 77.9% +/- 6.4% to 114.0% +/- 8.1% (average +/- standard deviation). The simple and rapid method may be used to routinely determine organochlorine pesticides in TCM.
本文描述了一种简单高效的同时气相色谱（GC）测定中药中18种有机氯农药[四氯硝基苯、六氯苯、α-六六六（BHC）、五氯硝基苯（PCNB）、γ-六六六、七氯、艾氏剂、甲基五氯苯基硫醚、β-六六六、δ-六六六、环氧七氯、α-硫丹、反式氯丹、顺式氯丹、p,p'-二氯二苯二氯乙烯、o,p'-滴滴涕、p,p'-滴滴滴和p,p'-滴滴涕]的方法。该方法采用超声提取和硫酸处理作为净化方法。样品检测通过GC-电子捕获检测进行。进行了一系列实验以优化最终预处理条件[丙酮-石油醚（1:1）作为提取溶剂，超声处理15分钟，分三步，用含10%水的浓硫酸进行硫酸处理]。除α-硫丹的加标水平为20、100和200 ppb外，对每种有机氯农药在10、50和100十亿分之一（ppb）的加标水平下进行回收率研究。回收率范围为77.9%±6.4%至114.0%±8.1%（平均值±标准差）。该简单快速的方法可用于常规测定中药中的有机氯农药。
