高效液相色谱-质谱法测定香姜中有机氯农药残留

目的]建立高效液相色谱-质谱法(HPLC-MS)测定香姜中有机氯农药残留分析方法。方法]采用正己烷-丙酮(4∶1)超声提取,过滤,盐析,干燥,经弗洛里硅土柱净化,用丙酮+正己烷(10+90)洗脱,用高效液相色谱-质谱联用法检测香姜中有机氯农药残留。结果]试验表明,有机氯农药标准的线性范围2~50μg/L,相关系数r均在0.99以上,在5、10、20μg/L加标水平下,平均回收率分别为80.0%~95.7%、82.4%~97.2%和83.6%~98.3%;相对标准偏差(RSD)分别为4.2%~9.8%、1.8%~9.4%和2.6%~8.8%。方法检出限(信噪比S/N≥3)均为1μg/kg,方法定量下限(信噪比S/N≥10)均为5μg/kg。结论]该方法简单、快速、准确,灵敏度和精密度好,适合香姜中有机氯农药残留的测定。

Determination of Organochlorine Pesticides Residues in Ginger by HPLC-MS

Method] To establish a detection method for the organochlorine pesticides residues in ginger by high liquid chromatograpy-mass spectrometry (HPLC-MS).Method] Ultrasonic extraction was carried out by n-hexane-acetone (4∶1).After filtration,salting out and drying,florida silica column was used for purification;and acetone + n-hexane (10 +90) was used for elution.Organochlorine pesticides residues were detected in ginger by HPLC-MS in ginger.Result] The standard linear range of organochlorine pesticides was 2-50 μg/L;correlation coefficient r was above 0.99.The average recovery rates at three levels of 5,10 and 20 μg/L were 80.0％-95.7％,82.4％-97.2％ and 83.6％-98.3％,respectively.Their relative standard deviations (RSD) were 4.2％-9.8％,1.8％-9.4％ and 2.6％-8.8％,respectively.The detection limit (S/N≥3) was 1 pg/kg;and the quantitation limit (S/N≥10) was 5 μg/kg.Conclusion] This method is simple,rapid,accurate and sensitive,and is suitable for the determination of organochlorine pesticides residues in ginger.