title: Multi-residue analysis of 26 organochlorine pesticides in Alpinia oxyphylla by GC-ECD after solid phase extraction and acid cleanup.
abstract: A simple and effective multi-residue method was developed and validated for the analysis of 26 organochlorine pesticide residues in Alpinia oxyphylla by a gas chromatography with an electron capture detector (GC-ECD). The target pesticides were extracted by sonication and cleaned up with florisil solid phase extraction and sulphuric acid. Some crucial parameters, including extraction solvent and time, sorbent type, elute solvent and concentration of sulphuric acid were optimized to improve the performance of sample preparation procedure. The optimized method gave high sensitivity with detection limit ranging from 0.1 to 2.0μg/kg. Matrix-matched calibration was employed for the quantification, and a wide linear range (from 1.0 to 1000μg/kg) with r(2) values ranging from 0.9971 to 0.9998 was obtained. For the majority of the tested pesticides, the average recoveries were in acceptable range (between 70% and 110%) with relative standard deviation values below 15.0%. Matrix effect was evaluated for target compounds through the study of ratio of peak area obtained in the solvent and blank matrix. The proposed method was applied to simultaneously analyze 26 pesticides in 55 batches of Alpinia oxyphylla samples. 3 samples were found to be positive with four pesticides (α-BHC, quintozene, trans-chlordane and op'-DDD), which were confirmed by gas chromatography-mass spectrometry (GC-MS) in selective ion monitoring (SIM) mode.
authors.affiliation: Hainan Branch Institute of Medicinal Plant Development, Chinese Academy of Medical Sciences & Peking Union Medical College, Wanning 571533, China.
authors.forename: Xiangsheng
authors.initials: X
authors.lastname: Zhao
authors.affiliation: Hainan Branch Institute of Medicinal Plant Development, Chinese Academy of Medical Sciences & Peking Union Medical College, Wanning 571533, China.
authors.forename: Yakui
authors.initials: Y
authors.lastname: Zhou
authors.affiliation: Institute of Medicinal Plant Development, Chinese Academy of Medical Sciences & Peking Union Medical College, Beijing 100193, China.
authors.forename: Weijun
authors.initials: W
authors.lastname: Kong
authors.affiliation: Hainan Branch Institute of Medicinal Plant Development, Chinese Academy of Medical Sciences & Peking Union Medical College, Wanning 571533, China.
authors.forename: Bao
authors.initials: B
authors.lastname: Gong
authors.affiliation: Hainan Branch Institute of Medicinal Plant Development, Chinese Academy of Medical Sciences & Peking Union Medical College, Wanning 571533, China.
authors.forename: Deli
authors.initials: D
authors.lastname: Chen
authors.affiliation: Hainan Branch Institute of Medicinal Plant Development, Chinese Academy of Medical Sciences & Peking Union Medical College, Wanning 571533, China; Institute of Medicinal Plant Development, Chinese Academy of Medical Sciences & Peking Union Medical College, Beijing 100193, China. Electronic address: jhwei@implad.ac.cn.
authors.forename: Jianhe
authors.initials: J
authors.lastname: Wei
authors.affiliation: Hainan Branch Institute of Medicinal Plant Development, Chinese Academy of Medical Sciences & Peking Union Medical College, Wanning 571533, China; Institute of Medicinal Plant Development, Chinese Academy of Medical Sciences & Peking Union Medical College, Beijing 100193, China. Electronic address: yangmeihua15@hotmail.com.
authors.forename: Meihua
authors.initials: M
authors.lastname: Yang
mesh_terms: D000143:Acids / Q000302:isolation & purification*; D032429:Alpinia / Q000737:chemistry*; D002849:Chromatography, Gas / Q000379:methods*; D006843:Hydrocarbons, Chlorinated / Q000032:analysis*; D010573:Pesticide Residues / Q000032:analysis*; D052617:Solid Phase Microextraction / Q000379:methods*
chemical_list: D000143:Acids; D006843:Hydrocarbons, Chlorinated; D010573:Pesticide Residues
keywords: Alpinia oxyphylla; Gas chromatography-electron capture detection; Organochlorine pesticides; Solid-phased extraction