GC-MS测定纺织品中有机磷农残含量检测方法研究

本实验在模拟人体环境下,利用人工汗液对生态纺织品中的有机磷农药残留进行提取,用GC/MS联用进行测定,采用外标法定量。实验过程中用21种农药混标,确定实验条件后(萃取时间25 min、萃取温度为室温、吸附时间3.5 min、Na2SO4以及pH为7),进行方法重现性、线性范围和检测限试验。发现重现性好,RSD值在1.56%~24.18%之间;线性良好,其中乙拌磷线性范围10~350 ppb,乙基溴硫磷50~500 ppb,丙溴磷20~500 ppb,另外还有烯虫磷、速灭磷、马拉硫磷、喹硫磷、毒虫畏5种有机磷的线性范围是0.1~350 ppb,二嗪磷、倍硫磷2种线性范围0.1~200 ppb,甲基对硫磷、乙基对硫磷2种0.1~500 ppb,敌敌畏、三唑磷2种100~350 ppb,检测限均低于20μg/L。对实际样品(100%棉织物)进行了加标回收实验,平行测量3次的相对平均偏差在0.75%~13.92%之间,回收率在84.96%~110.91%之间,这说明SPME-GC-MSD法用于检测纺织品中有机磷农药残留,有很好的重现性和精密度,可进行纺织品中有机磷农药残留的定量检测分析。

Study on GC-MS Determination Method for Detection Oforganophosphorus Pesticide Residues in Textiles

The experiment using the artificial sweat, which simulated the human environment, to extract the organophosphorus pesticide residues of ecological textiles, and then using GC/MS to determine the quantitative with the external standard method. After determining the experimental conditions （extraction time： 25 min, extraction temperature： room temperature, adsorption time： 3.5 min, Na2SO4 and pH：7）, the experiment using Pesticide Mix 21 to carry out the method reproducibility, linearity range and detection limit. The method was proved to be good in reproducibility and linearity - RSD was between 1.56 % and 24.18 %; Disulfoton linear range of 10-350 ppb, Bromopbos ethyl 50-500 ppb, Profenofos 20-500 ppb; in addition, five kinds of organic phosphorus linear, which include Propetamphos, Mevinphos, Malathion, Quinalphos, Chlorfenvinphos, range of 0.1-350 ppb; Diazinon and fenthion linear range of 0.1-200 ppb; Methyl parathion and Ethyl parathion 0.1-500 ppb; DDVP and phentriazophos 100-350 ppb. All the detection limit were below 20 μg/L. The actual sample （100 % cotton fabric） were gained by spiked recovery experiments, the relative average deviation of three parallel measurements was between 0.75 %-13.92 %, and the recovery was between 84.96 %-110.91%. The indicates that the SPME-GC-MSD method for the detection of organophosphorus pesticide residues in textiles, has good reproducibility and precision, can be quantitatively detected in analyzing organophosphorus pesticide residues.