色谱

色谱

• 研究论文 • 上一篇    下一篇

气相色谱-双柱双电子捕获检测器测定土壤及沉积物中23种有机氯农药

朱恒怡1, 柳文媛1,2*, 丁曦宁3, 赵永刚3   

  1. 1. 中国药科大学药物分析教研室, 江苏 南京 210009; 2. 药物质量与安全预警教育部重点实验室(中国药科大学), 江苏 南京 210009; 3. 江苏省环境监测中心, 江苏 南京 210036
  • 收稿日期:2011-03-06 修回日期:2011-05-03 出版日期:2011-08-28 发布日期:2011-09-28
  • 通讯作者: 柳文媛,副教授,研究方向为现代药物分析. Tel: (025)83271038

Determination of 23 organochlorine pesticides in soil and sediment by gas chromatography coupled with dual columns and dual electron capture detectorsorganochlorine pesticides in soils and sediments by Microwave Extraction and GC coupled with dual-column and dual-ECD

ZHU Hengyi1, LIU Wenyuan1,2*, DING Xining3, ZHAO Yonggang3   

  1. 1. Department of Pharmaceutical Analysis, China Pharmaceutical University, Nanjing 210009, China; 2. Key Laboratory of Drug Quality Control and Pharmacovigilance of Ministry of Education, China Pharmaceutical University, Nanjing 210009, China; 3. Jiangsu Environmental Monitoring Centre, Nanjing 210036, China
  • Received:2011-03-06 Revised:2011-05-03 Online:2011-08-28 Published:2011-09-28

PDF

443

被引次数

11

摘要： 建立了微波萃取,弗罗里硅土固相萃取柱及铜粉除硫净化,双柱双电子捕获检测器(ECD)-气相色谱法(GC)测定5种不同质地土壤及5处不同来源沉积物中的23种有机氯农药(OCPs)。采用内标法定量,在0.005～0.5 mg/L的质量浓度范围内,替代物和各种农药标准品的线性相关系数(r2)均大于0.997。5种土壤及5处沉积物中23种OCPs的平均加标回收率分别为50%～119%和52%～120%,相对标准偏差分别为0.9%～16.1%(n=6)和0.3%～28.4%(n=6),检出限为0.00005～0.0005 mg/kg。结果表明,该方法重现性好、灵敏度高、线性关系好,可以满足简便、快速、准确测定农药残留的要求,可大范围推广使用。

关键词: 沉积物, 双柱双电子捕获检测器气相色谱法, 土壤, 微波萃取, 有机氯农药

Abstract: Gas chromatography (GC) coupled with dual columns and dual electron capture detectors (ECD) was established to determine 23 organochlorine pesticides in 5 soil and 5 sediment samples. Microwave assisted extraction and solid phase extraction with a Florisil column and sulfur cleanup with copper powder were used in sample pre-processing. Chromatographic analysis was performed on DB-XLB and DB-1701 capillary columns by internal standard method. This method showed good extraction efficiency, high sensitivity and good reproducibility. In the same linear range of 0.005~0.5 mg/L of 23 pesticides, the correlation coefficients were higher than 0.997. The average spiked recoveries were 50%~119% with the relative standard deviations (RSDs) of 0.9%~16.1% (n=6) in 5 soil samples, and were 52%~120% with RSDs of 0.3%~28.4% (n=6) in 5 sediment samples, respectively. The detection limits were 0.00005~0.0005 mg/kg. The results indicate that this method is suitable for the determination of the 23 organochlorine pesticides in soil and sediment samples.

Key words: organochlorine pesticides, sediment, soil, gas chromatography coupled with dual columns and dual electron capture detectors, microwave extraction