目的:建立检测果实类中药材中41种有机磷农药残留的气相色谱分析方法。方法:样品以乙腈为提取剂超声提取,提取液经PSA固相萃取柱净化,正己烷∶丙酮(1∶1)洗脱,采用ZB1701毛细管色谱柱分离,GC-FPD检测器进行检测。结果:41种有机磷农药在50-500μg/kg范围内线性关系良好,相关系数(r)为0.9914-0.9987之间。分别对5种果实类中药材进行50、100、500μg/kg 3个浓度水平的添加回收率试验,平均回收率大部分在70%-120%之间,相对标准偏差(RSD)小于15%。方法的定量限大多低于50μg/kg,符合农药残留痕量测定要求。结论:本方法准确度高,灵敏度好,操作简便。
Objective: To establish the gas chromatographic method for the determination of 41 organophosphorus pesticides in fruit Chinese medicines. Methods: The sample were extracted with acetonitril, cleaned up by PSA solid phase extraction column, eluted by n-hexane∶acetme(1∶1), and finally determinated by gas chromatographic-flame photometric detection(GC-FPD) in ZB1701 capillary column. Results: The standard calibration curves for 41 organophosphorus pesticides showed high correlation coefficient(r=0.9914-0.9987) over 50-500μg/kg. The average recoveries at the three fortification levels(50, 100, 500μg/kg) were between 70% and 120% with the relative standard deviation(RSD) under 15%. The limits of quantification(LOQ) were less than 50μg/kg. Conclusion: It is indicated that the method develop in this study is easier, more sensitive and has a better purification effect.