色谱

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高效液相色谱法同时检测棉织品中的9种有机氯农药残留

张翔,廖青,张焱

  

  1. School of Materials Science & Engineering, Beijing Institute of Clothing Technology, Beijing 100029, China
  • 收稿日期:2006-09-15 修回日期:2007-02-06 出版日期:2007-05-30 发布日期:1985-09-25
  • 通讯作者: 廖青

Simultaneous Determination of Nine Organochlorine Pesticide Residues in Textile by High Performance Liquid Chromatography

ZHANG Xiang, LIAO Qing, ZHANG Yan   

  1. School of Materials Science & Engineering, Beijing Institute of Clothing Technology, Beijing 100029, China
  • Received:2006-09-15 Revised:2007-02-06 Online:2007-05-30 Published:1985-09-25

摘要:

建立了高效液相色谱-二极管阵列检测器测定棉织品中9种有机氯农药含量的方法。采用丙酮-石油醚超声萃取法提取纺织品中的农药残留物,采用填料粒径为5 μm的ODS色谱柱,甲醇-磷酸水溶液(pH 2.27)体系为流动相,梯度洗脱,柱温30 ℃,流速0.8 mL/min,在波长230 nm下检测。9种农药在0.5~10 mg/L范围内峰面积与其浓度具有良好的线性关系(r2>0.9988)。该法简便、准确、灵敏度高、重现性好、回收率高(85.5%~99.6%),可用于纺织品中有机氯杀虫剂和除草剂含量的测定。

关键词: 高效液相色谱, 农药残留, 生态纺织品 , 有机氯农药

Abstract:

A method for the simultaneous determination of pesticide and herbicide residues in cotton textile by high performance liquid chromatography coupled with diode array detector (HPLC-DAD) has been established. The pesticides and herbicides determined were 2,4-dichlorophenoxy (2,4-D), 2-methyl-4-chlorophenoxy acetic acid (MCPA), dichlorprop, mecoprop, 2,4,5-trichlorophenoxy (2,4,5-T), 2-methyl-4-chlorophenoxy butyric acid (MCPB), β-endosulfan, methoxychlor and 2,2-bis(p-chlorophenyl)-1,1-dichloroethene (DDE). Pesticide and herbicide residues in cotton products were extracted with acetone-petroleum ether by ultrasonic instrument. The extract was analyzed using an SGE C18 column with a linear gradient elution (methanol-phosphoric acid as mobile phase at a flow rate of 0.8 mL/min) and ultraviolet detection at 230 nm. The linear range was 0.5-10 mg/L, and the correlation coefficients were all greater than 0.9988. By using acetone-petroleum ether(4∶1, v/v) as solvent, the recoveries of nine organochlorine pesticides and herbicides at spiked levels of 0.5-2 mg/kg were 85.5%-99.6%. The limits of detection (S/N=3) were 0.05 mg/kg except MCPB, β-endosulfan, methoxychlor and DDE that were 0.10 mg/kg. This method is of high accuracy, easy operation, satisfactory recoveries and good reproducibility. It could be used for the determination of the nine pesticides and herbicides in textile.

Key words: eco-textile , organochlorine pesticides, pesticide-residues, high performance liquid chromatography (HPLC)