气相色谱-串联质谱法测定原料类果酱中百菌清残留量

Determination of chlorothalonil residues in raw jam by gas chromatography-tandem mass spectrometry

中文关键词:  原料类果酱  百菌清  农药残留  气相色谱-串联质谱法

英文关键词:raw jam  chlorothalonil  pesticide residues  gas chromatography-tandem mass spectrometry

中文摘要:

      目的 建立气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry, GC-MS/MS)测定原料类果酱中百菌清农药残留的检测方法。方法 样品经8 mL去离子水水化, 采用乙腈提取, 加入4 g氯化钠盐析, 4200 r/min离心8 min。上清液经氟罗里硅土固相萃取柱净化, 使用正己烷-丙酮混合溶液(9:1, V:V)洗脱, 气相色谱-串联质谱仪测定, 外标法定量。结果 标准曲线在5~250 ng/mL范围内线性良好, 相关系数大于0.99。百菌清的定量限为0.01 mg/kg; 在0.01~0.10 mg/kg浓度范围的加标实验中, 回收率为83.0%~116.8%, 精密度为3.7%~10.3%。结论 该方法操作简便、结果准确, 适用于原料类果酱中百菌清残留的测定。

英文摘要:

      Objective To establish a method for quantitative determination of chlorothalonil pesticide residue in raw jam materials by gas chromatography-tandem mass spectrometry (GC-MS/MS). Methods The sample was hydrated by 8 mL of deionized water, extracted by using acetonitrile, salted out with 4 g sodium chloride, centrifuged at 4200 r/min for 8 min. The supernatant was cleaned up by a florisil solid phase extraction column and eluted by n-hexane-acetone mixture (9:1, V:V), the analytes were determined by GC-MS/MS and quantified by external standard method. Results The standard curve had a good linear relationship in the range of 5?250 ng/mL, with the correlation coefficient was greater than 0.99. The limit of quantification of chlorothalonil was 0.01 mg/kg; the recoveries varied from 83.0% to 116.8% and the relative standard deviations varied from 3.7% to 10.3% at spiked levels of 0.01?0.10 mg/kg. Conclusion This method is simple, convenient, accurate and suitable for detection of chlorothalonil residue in raw jam materials.