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

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

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5um的ODS色谱柱，甲醇-磷酸水溶液（pH2．27）体系为流动相，梯度洗脱，柱温30℃，流速0．8mL／min，在波长230nm下检测。9种农药在0．5—10mg／L范围内峰面积与其浓度具有良好的线性关系（r^2〉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。

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-trichiorophenoxy （2,4,5-T）, 2-methyl-4-chlorophenoxy butyric acid （ MCPB ）, β-en- dosulfan, methoxychlor and 2,2-bis （ p-chiorophenyl ） -1,1-dichioroethene （ 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. 998 8. 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, methoxychior 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.