改进QuEChERS-液质联用法测定黄精中23种农药残留

Improved QuEChERS liquid chromatography-mass spectrometry for the determination of 23 pesticide residues in Polygonatum sibiricum

建立黄精中氧乐果、多菌灵、噻虫嗪等23种农药残留的QuEChERS快速样品处理结合液相色谱-串联质谱检测方法,对净化条件、质谱条件等进行了优化。样品用1%乙酸乙腈提取,用900 mg无水硫酸镁、300 mg N-丙基乙二胺、300 mg十八烷基硅烷键合硅胶和100 mg硅胶净化。结果表明,23种农药多残留的回收率均在75.61%~114.52%,线性关系良好,相关系数在0.995 5~0.999 9,相对标准偏差小于9.99%,测定低限均不超过《中华人民共和国药典》(2020年版)规定的定量限。

A QuEChERS rapid sample processing combined with liquid chromatography-tandem mass spectrometry detection method was established for 23 pesticide residues in Polygonatum sibiricum,including omethoate,carbendazim,and thiamethoxam.Purification and mass spectrometry conditions were optimized.The sample was extracted with 1% acetonitrile acetate and purified with 900 mg anhydrous magnesium sulfate,300 mg N-propylethylenediamine,300 mg octadecylsilane bonded silica gel,and 100 mg silica gel.The results showed that the recovery rates of 23 pesticide residues were all between 75.61% and 114.52%,with a good linear relationship.The correlation coefficient was between 0.995 5 and 0.999 9,and the relative standard deviation was less than 9.99%.The lower limit of determination was not exceed the quantitative limit specified in the Pharmacopoeia of the People′s Republic of China(2020 version).