首页|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

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

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  • NETL
  • NSTL
  • 万方数据
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 500 μL、1000 μL、1500 μL(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500 μL、1000 μL、1500 μL(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Waters XEVO TQMS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。
Determination of 35 Prohibited Pesticides in Panax Ginseng by Gas Chromatography-Triple Quadrupole Tandem Mass Spectrometry and High-performance Liquid Chromatography-tandem Mass Spectrometry
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 500 μL,1000 μL,1500 μL 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 500 μL、1000 μL、1500 μL 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.

gas chromatography-triple quadrupole tandem mass spectrometryhigh-performance liquid chromatography-tandem mass spectrometryprohibit pesticide residuesdirect extraction methodPanax Ginseng

谢春晓、陈海明、陈小锐、李程瑶、余静怡

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广东省药品监督管理局事务中心,广东 广州 510000

清远市食品药品检验所,广东 清远 511517

气相色谱-三重四极杆串联质谱法 高效液相色谱-串联质谱检法 禁用农药残留物 直接提取法 人参

2024

10.3969/j.issn.1007-1865.2024.08.044

广东化工
广东省石油化工研究院

广东化工

影响因子：0.288
ISSN：1007-1865
年,卷(期)：2024.51(8)