气相色谱串联质谱测定炒白术中氟虫腈类残留的不确定度评定

Uncertainty Assessment of Fipronil Residues in Frying by Gas Chromatography Tandem Mass Spectrometry

本研究按照2020版《中国药典》四部通则2341第五法对炒白术中氟虫腈类农药残留量的不确定度进行评定。本文通过建立计算模型,分析不确定度各分量来源,计算在药典规定的限制含量水平下的不确定度。结果表明,在药典限制水平时,氟虫腈、氟虫腈亚砜、氟甲腈、氟虫腈砜的扩展不确定度分别为0.0035 mg/kg、0.0045 mg/kg、0.0040 mg/kg、0.0040 mg/kg。由于该方法测定32种农药残留量的不确定度主要来源是标准曲线的配制与拟合,因此在配制标准溶液的过程中,检验人员要选择合适的稀释方法及测量仪器,正确使用各种量具和测量仪器。同时,应定期检查和校准各种量具和测量仪器设备。

The uncertainty of fipronil pesticide residues in whitening was assessed according to the fifth method of four General Rules 2341 of Chinese Pharmacopoeia 2020 edition.By analyzing the component sources of uncertainty,calculate the uncertainty at the level of limit content specified in the Pharmacopoeia.The results showed that At the limit level of the pharmacopoeia,the expanded uncertainty of fipronil,fipronil sulfoxide,fipronil,and fipronil sulfone were 0.0035 mg/kg,0.0045 mg/kg,0.0040 mg/kg,and 0.0040 mg/kg,respectively.The main source of uncertainty in the determination of 32 pesticide residues is the preparation and fitting of standard curve.Therefore,in the process of preparing standard solution,the inspectors should choose the appropriate dilution method and measuring instruments,and correctly use a variety of measuring tools and measuring instruments.At the same time,various measuring tools and measuring instruments should be checked and calibrated regularly.