Zhao Chunjie, Hao Guiming, Li Huanxin, Chen Yingjie
Shenyang Pharmaceutical University, Shenyang 110016, People's Republic of China.
Biomed Chromatogr. 2002 Oct;16(7):441-5. doi: 10.1002/bmc.180.
A method involving the simultaneous extraction and separation of 12 organochlorine pesticides (OCPs) from Angelicae sinensis was developed using supercritical fluid extraction (SFE). The pesticides in the study were alpha-, beta-, gamma- and delta-benzene hexachloride, PCNB (pentachloro- nitrobenzene), PCA (pentachloroaniline), HEPT (heptachlor), MPCPS (methyl-pentachlorophenyl sulfide), pp'-DDE [1,1-dichloro-2,2-bis (p-chlorophenyl) ethylene], op'-DDT [1,1,1,-trichloro-2-(o-chlorophenyl)-2-(p-chlorophenyl) ethane], pp'-DDD [1,1-dichloro-2,2-bis(p-chlorophenyl) ethane], and pp'-DDT [1,1,1,-trichloro-2,2-bis (p-chlorophenyl)ethane]. The extraction conditions were optimized as follows: pure CO(2), extraction pressure 15 MPa, extraction temperature 60 degrees C, extraction time 20 min, and flow-rate 1.5 mL/min. A GC method with electron capture detection was employed to determine the OCPs in Angelicae sinensis. An HPLC method was developed for the quantitative determination of active constituents. The SFE provided high decontamination rate of OCPs and low loss of active constituents in Angelicae sinensis.
建立了一种采用超临界流体萃取（SFE）同时从当归中萃取和分离12种有机氯农药（OCPs）的方法。研究中的农药有α-、β-、γ-和δ-六六六、五氯硝基苯（PCNB）、五氯苯胺（PCA）、七氯（HEPT）、甲基五氯苯基硫醚（MPCPS）、p,p'-滴滴伊[1,1-二氯-2,2-双（对氯苯基）乙烯]、o,p'-滴滴涕[1,1,1-三氯-2-（邻氯苯基）-2-（对氯苯基）乙烷]、p,p'-滴滴滴[1,1-二氯-2,2-双（对氯苯基）乙烷]以及p,p'-滴滴涕[1,1,1-三氯-2,2-双（对氯苯基）乙烷]。萃取条件优化如下：纯二氧化碳，萃取压力15兆帕，萃取温度60℃，萃取时间20分钟，流速1.5毫升/分钟。采用带有电子捕获检测的气相色谱法测定当归中的有机氯农药。开发了一种高效液相色谱法用于活性成分的定量测定。超临界流体萃取法对当归中有机氯农药的去除率高，且活性成分损失低。
