气相色谱-三重四极杆质谱法测定人参中22种有机氯农残
目的 建立气相色谱-三重四级杆质谱法(gas chromatography-triple quadruple mass spectrometry, GC-MS/MS)测定人参中22种有机氯农残的分析方法。方法 参考《中华人民共参和国药典》2015年版, 选择样品前处理方法, 优化色谱质谱条件, 建立22种有机氯农残的GC-MS/MS检测方法。结果 22种有机氯农药在2.5~1000 μg/L范围内, 线性关系良好, 线性相关系数(r2)为0.9992~0.9999; 加标回收率良好为81.40%~118.29%, 相对标准偏差(relative standard deviation, RSD)值为9.25%; 重复性良好, RSD值为1.46%~3.28%; 检出限为0.01~2.57 μg/kg, 定量限为0.03~8.63 μg/kg。结论 该方法能满足中国药典的检测要求, 检测结果通过了中国食品药品检定研究院开展的人参中22种有机氯农残能力验证项目, 表明本实验室具备该项目的检测能力, 对人参及其它中药材中有机氯农残的监控, 保障人们的安全食用和身体健康具有积极意义。
Objective To establish a method for the simultaneous determination of 22 kinds of organochlorine pesticide residues in ginseng by gas chromatography-triple quadruple mass spectrometry (gas chromatography-triple quadruple mass spectrometry, GC-MS/MS). Methods Refer to the pharmacopoeia of the people’s republic of China (2015), the method of the determination of 22 kinds of organochlorine pesticide residues in ginseng by GC-MS/MS was created by the selection of sample pretreatment methods and the optimization of gas chromatography and mass spectrometry condition. Results The 22 kinds of organochlorine pesticide residues had a good linear relationship in the range of 2.51000 μg/L, and the linear correlation coefficients (r2) were 0.99920.9999. The recoveries were good, which were between 81.40%118.29%, and the corresponding RSD value was 9.25%. The repeatability was good, and the corresponding RSD values were 1.46%3.28%. The limit of detection and quantification were 0.012.57 μg/kg and 0.038.63 μg/kg. Conclusion This method could meet the requirements of the pharmacopoeia of the people’s republic of China (2015), and the results have passed the proficiency test of 22 kinds of organochlorine pesticide residues which is carried out by national institutes for food and drug control of China. The results indicate that our laboratory has the detectability for the proficiency test which is positive to the monitoring of organochlorine pesticide residues in ginseng and other Chinese medical herbs, as well as the safe taking and good health of people.
标题:气相色谱-三重四极杆质谱法测定人参中22种有机氯农残
英文标题:Determination of 22 kinds of organochlorine pesticide residues in ginseng by gas chromatography-triple quadruple mass spectrometry
作者:
钱冲 北京市理化分析测试中心,有机材料检测技术与质量评价北京市重点实验室
胡光辉 北京市理化分析测试中心,有机材料检测技术与质量评价北京市重点实验室;北京市科学技术研究院分析测试技术重点实验室
张梅 北京市理化分析测试中心,有机材料检测技术与质量评价北京市重点实验室;北京市科学技术研究院分析测试技术重点实验室
白云 北京市理化分析测试中心,有机材料检测技术与质量评价北京市重点实验室
勾新磊 北京市理化分析测试中心,有机材料检测技术与质量评价北京市重点实验室
高峡 北京市理化分析测试中心,有机材料检测技术与质量评价北京市重点实验室;北京市科学技术研究院分析测试技术重点实验室
刘伟丽 北京市理化分析测试中心,有机材料检测技术与质量评价北京市重点实验室;北京市科学技术研究院分析测试技术重点实验室
中文关键词:人参,气相色谱-三重四极杆质谱法,有机氯农残,能力验证,
英文关键词:ginseng,gas chromatography-triple quadruple mass spectrometry,organochlorine pesticide residues,proficiency test,
发表日期:2019-11-10
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