QuEChERS-高效液相色谱-串联质谱法测定滇黄精中6种农药残留量

Determination of 6 kinds of pesticide residues in Polygonatum kingianum Coll. et Hemsl. by QuEChERS-high performance liquid chromatography-tandem mass spectrometry

中文关键词:  QuEChERS  高效液相色谱-串联质谱法  滇黄精  农药残留

英文关键词:QuEChERS  high performance liquid chromatography-tandem mass spectrometry  Polygonatum kingianum Coll. et Hemsl.  pesticide residues

中文摘要:

      目的 建立QuEChERS-高效液相色谱-串联质谱法同时测定滇黄精中6种农药残留量的分析方法。方法 滇黄精样品粉碎后经乙酸乙腈溶液(1:99, V:V)均质提取, 采用无水硫酸镁、乙二胺-N-丙基硅烷和十八烷基键合硅胶吸附剂净化, 经高效液相色谱-串联质谱仪在正离子模式下扫描分析滇黄精中6种农药残留量, 采用空白基质匹配外标法定量。结果 6种农药在2~100 ng/mL的质量浓度范围内线性关系良好, 决定系数均大于0.995; 检出限为0.07~0.46 μg/kg, 定量限为0.14~0.91 μg/kg。在3个加标水平下, 6种农药整体平均回收率为90.4%~100.7%; 相对标准偏差(n=6)为0.8%~2.3%, 均小于15%。结论 本方法快速、高效、准确, 精密度和灵敏度高, 能满足滇黄精中6种农药残留定量分析要求, 可为监测滇黄精食用质量安全与药用质量均一性提供基础技术支撑。

英文摘要:

      Objective To establish a method for simultaneous determination of 6 kinds of pesticide residues in Polygonatum kingianum Coll. et Hemsl. by QuEChERS-high performance liquid chromatography-tandem mass spectrometry. Methods The pulverized Polygonatum kingianum Coll. et Hemsl. samples were homogeneously extracted with ethyl acetate-acetonitrile solution (1:99, V:V). Magnesium sulfate anhydrous, primary secondary amine and octadecylsilane bonded silica gel sorbents were used for purification. The 6 kinds of pesticide residues in Polygonatum kingianum Coll. et Hemsl. were analyzed by high performance liquid chromatography-tandem mass spectrometry under positive electrospray ionization mode, and quantified via matrix-matched external standard method. Results The 6 kinds of pesticides exhibited good linear relationships within the mass concentration range of 2–100 ng/mL, with all coefficients of determination greater than 0.995. The limits of detection were 0.07–0.46 μg/kg, and the limits of quantitation were 0.14–0.91 μg/kg. At 3 spiked concentration levels, the overall average recoveries of the 6 kinds of pesticides ranged from 90.4% to 100.7%, and the relative standard deviations (n=6) were 0.8%–2.3% (all less than 15%). Conclusion This method is rapid, efficient, accurate with favorable precision and sensitivity. It can meet the requirements for quantitative analysis of the 6 kinds of pesticide residues in Polygonatum kingianum Coll. et Hemsl., and provides fundamental technical support for monitoring the edible quality safety and medicinal quality consistency of Polygonatum kingianum Coll. et Hemsl.