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采用高效液相色谱(HPLC)法,对5种有机磷农药(OPPs)同时进行分离、制备,对其紫外检测波长、流动相比例进行了优化,对方法的精密度和最小检出限进行了考查。结果表明,以甲醇:水(70:30,V/V)作为流动相、波长为210nm、流速为1.0mL/min等梯度洗脱条件下,HPLC完全可以分离5种OPPs化工产品(氧乐果、敌百虫、敌敌畏、马拉硫磷、甲拌磷),制得5种单一有机磷标准物质。该方法的最小检出限除敌百虫(42.72 ng)较高外,余者皆在1.05~2.28ng之间;制备浓度在30.5~1066.3μg/mL之间;纯度皆达97%以上;回收率除氧乐果以外,余者皆在99.89%~120.04%之间;相对标准偏差在0.38%~6.40%之间,精密度高。该方法适用于有机磷农药的分析检测与制备。
Five kinds of organophosphorus pesticides (OPPs) were isolated and prepared simultaneously by high performance liquid chromatography (HPLC). The UV detection wavelength and mobile phase ratio were optimized. The precision and minimum detection limit of the method were optimized test. The results showed that under the conditions of isocratic elution with methanol: water (70:30, V / V) as mobile phase, wavelength of 210 nm and flow rate of 1.0 mL / min, , Trichlorfon, dichlorvos, malathion, phorate), five kinds of single organophosphorus standard substances were prepared. The minimum detectable limit of this method was higher than that of trichlorfon (42.72 ng) except for 1.05 ~ 2.28 ng, with the purity of 30.5 ~ 1066.3 μg / mL and the purity of both was above 97% Rate of Omethoate, the remaining were between 99.89% ~ 120.04%; relative standard deviation between 0.38% ~ 6.40%, high precision. The method is suitable for the detection and preparation of organophosphorus pesticides.