摘要: |
目的:采用气相色谱-串联质谱法(GC-MS)分析技术建立定性和定量检测中药材茯苓中25种禁用农药残留的方法。方法:以乙腈为提取溶剂,对干燥茯苓样品进行提取、净化、浓缩等预处理后,经气相色谱-三重四极杆串联质谱分析测定,并用内标法定量。结果:茯苓中25种禁用农药在1~100 ng/ml范围内具有良好的线性关系,相关系数均在0.9900以上;检出限在0.00040~0.0100 mg/kg;定量限在0.000667~0.0333 mg/kg;以上检测均符合农药残留的检测要求。加标回收实验的平均加标率为70.1%~123.3%,加标率和加标样品的重复性验证结果也均符合标准要求。18批茯苓样品均未检出25种农药残留。结论:该方法简便快速、灵敏度高、重现性好,可适用于多种中药材中禁用农药残留的检测。 |
关键词: 气相色谱-串联质谱法 禁用农药 中药材 茯苓 |
DOI: |
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Determination of forbidden pesticide residue in Chinese medicinal material Poria cocos based on gas chromatography-mass spectroscopy |
YUAN Nong,DU Juan,LONG Huiling |
(Hunan Center for Drug Evaluation and ADR Monitoring,Changsha 410013,Hunan,China) |
Abstract: |
Objective:To establish a method for qualitative and quantitative determination of the residue of 25 forbidden pesticides in the Chinese medicinal material Poria cocos using gas chromatography-mass spectroscopy.Methods:With acetonitrile as the extraction solvent,dried Poria cocos samples were pretreated by extraction,purification,and concentration,and then gas chromatography-triple quadrupole tandem mass spectrometry was used for analysis and determination,with the internal standard method for quantification.Results:The 25 forbidden pesticides in Poria cocos showed a good linear relationship within the range of 1-100 ng/mL,with a correlation coefficient of >0.9900.The limit of detection had a range of 0.00040-0.0100 mg/kg,and the limit of quantification had a range of 0.000667-0.0333 mg/kg.All the results above met the requirements for pesticide residue.The mean recovery rate was 70.1%-123.3%,and the results of recovery rate and repeatability also met the standard requirements.The residue of 25 pesticides was not detected in 18 batches of Poria cocos samples.Conclusion:This method is simple and rapid with high sensitivity and good repeatability and can be used for determining the residue of various forbidden pesticides in Chinese medicinal materials. |
Key words: gas chromatography-mass spectroscopy forbidden pesticide Chinese medicinal material Poria cocos |