气相色谱——三重四极杆串联质谱法及高效液相色谱——串联质谱检法测定人参中禁用农药残留物

Determination of 35 Prohibited Pesticides in Panax Ginseng by Gas Chromatography-Triple Quadrupole Tandem Mass Spectrometry and High-performance Liquid Chromatography-tandem Mass Spectrometry

目的:建立使用气相色谱-三重四极杆串联质谱法及高效液相色谱-串联质谱检法测定人参中禁用农药残留物的测定方法。方法:参照2020年版《中国药典》通则2341第五法4.1方式操作步骤,分别采用岛津气相色谱-串联质谱GC-MSTQ8040、高效液相色谱-串联质谱Waters XEVO TQMS进行检测分析。结果:对空白样品按低中高浓度分别加入混合对照品溶液500μL、1000μL、1500μL(添加浓度以灭线磷计分别为:0.04 mg/kg;0.08 mg/kg;0.12 mg/kg)后,按照文中前处理方法处理后,在岛津气相色谱-串联质谱GC-MSTQ8040上机,每个浓度平行3份样品考察回收率和RSD,结果显示,低中高浓度加标回收率分别为:86.83%~108.43%;91.39%~112.99%;88.47%~115.09%。,RSD分别为:0.54%~9.74%;2.24%~4.20%;1.07%~2.96%。回收率高,重现性好。对空白样品按低中高浓度分别加入混合对照品溶液500μL、1000μL、1500μL(添加浓度以灭线磷计分别为:0.1 mg/kg;0.2 mg/kg;0.3 mg/kg)后,按照文中前处理方法处理后,在高效液相色谱-串联质谱WatersXEVOTQMS上机,每个浓度平行3份样品考察回收率和RSD,结果显示,低中高浓度加标回收率分别为:74.33%~103.29%;72.55%~105.16%;81.54%~103.41%。RSD分别为:0.29%~6.01%;1.07%~8.32%;0.41%~7.74%。回收率高,重现性好。结论:该方法便捷,回收率和稳定性良好,适用于人参中禁用农药残留物的测定。

Objective:To establish a method for the determination of prohibited pesticide residues in ginseng using gas chromatography-triple quadrupole tandem mass spectrometry and high-performance liquid chromatography-tandem mass spectrometry.The method follows the operation steps of Section 4.1 of General Rule 2341 in the 2020 edition of the Chinese Pharmacopoeia.Shimadzu gas chromatography-tandem mass spectrometry GC-MSTQ8040 and high-performance liquid chromatography-tandem mass spectrometry Waters XEVO TQMS were used for detection and analysis.Result:Add 500μL,1000μL,1500μL mixed reference solutions to the blank samples at low,medium,and high concentrations.After adding concentrations of 0.04 mg/kg,0.08 mg/kg,and 0.12 mg/kg of phosphorus,according to the pre-treatment method mentioned in the article,the recovery rate and RSD were tested on three parallel samples of Shimadzu gas chromatography-tandem mass spectrometry GC-MSTQ8040 for each concentration.The results showed that the recovery rates of low,medium,and high concentrations were 86.83%~108.43%,respectively;91.39%~112.99%;88.47%~115.09%,The RSD is 0.54%~9.74%respectively;2.24%~4.20%;1.07%~2.96%.High recovery rate and good reproducibility.Add 500μL、1000μL、1500μL mixed reference solutions to the blank sample at low,medium,and high concentrations.After adding concentrations of 0.1 mg/kg,0.2 mg/kg,and 0.3 mg/kg of phosphorus,according to the pre-treatment method mentioned in the article,the recovery and RSD of each concentration were tested on three parallel samples using high-performance liquid chromatography tandem mass spectrometry Waters XEVO TQMS.The results showed that the recovery rates of low,medium,and high concentration spiked samples were 74.33%~103.29%,respectively;72.55%~105.16%;81.54%~103.41%.The RSD ranges from 0.29%to 6.01%;1.07%~8.32%;0.41%~7.74%.High recovery rate and good reproducibility.Conclusion:This method is fast,simple,with good recovery and stability,and is suitable for the determination of 35 prohibited pesticide residues in Panax Ginseng.