超高效液相色谱-串联质谱法测定拳参等5种人参中药材中24种农药残留  

Determination of 24 pesticide residues in 5 kinds of ginseng herbal medicines by Ultra-High Performance Liquid Chromatography-Triple Quadrupole Mass Spectrometry(UPLC-MS/MS)

作　　者：俞所银 虞成华[1] 徐红斌[1] YU Suoyin;YU Chenghua;XU Hongbin(Shanghai Institute of Quality Inspection and Technical Research,Shanghai 200233)

机构地区：[1]上海市质量监督检验技术研究院,上海200233

出　　处：《中国食品添加剂》2022年第10期213-222,共10页China Food Additives

基　　金：食品安全风险分级评价预警与现代监督执法技术的应用示范(2019YFC1606404)子课题:食品安全违法行为研判和违法案件的快速筛查技术应用示范研究(4-4)。

摘　　要：建立了拳参、人参、西洋参、北沙参和南沙参5种中药材中24种农药残留量的超高效液相色谱-串联质谱法的检测技术。样品采用1 %冰醋酸浸润、乙腈提取,QuEChERS净化。待测液经Phenomenx Kinetex C色谱柱(100*2.1mm,2.6μm)分离,含0.1%甲酸的5mM甲酸铵溶液和乙腈为流动相梯度洗脱,通过电喷雾离子源正离子(ESI^(+))方式离子化、多反应监测(MRM)模式测定,内标法定量。24种农药在0.05~100.0ng/g范围内有良好的线性关系(r>0.995),方法检出限(LOD,S/N=3)为0.05~5.0ng/g,方法定量限(LOQ,S/N>10)为0.15~15.0ng/g。在3个添加水平下,5种人参中药材回收率均在76.4%~117.7%之间,相对标准偏差(RSD)介于0.54%~10.21%之间。本方法灵敏度高、稳定性好、快速、准确,能够满足中药检测标准中面临的基质干扰问题。A method for the determination of 24 disable pesticide residues in 5 kinds of ginseng herbal medicines by Ultra-High Performance Liquid Chromatography-Triple Quadrupole Mass Spectrometry(UPLC-MS/MS)was established.Ginseng herbal medicines were Polygonum bistorta L,Panax ginseng C.A.Mey,Panax quiquefolium L,Radix Glehniae and Adenophore Radix,respectively.The samples were infiltrated by 1 % glacial acetic acid and extracted with acetonitrile,followed by purification of the QuEChERS sorbents.The filtrates were separated by the Phenomenx Kinetex Ccolumn(100*2.1mm,2.6μm)with gradient elution using 5mM ammonium formate solution containing 0.1% formic acid and acetonitrile as mobile phases,detected by electrospray ion source positive ion detection mode(ESI)and multiple reaction monitoring mode(MRM),quantified by the internal standard method.24 pesticide residues had good linear relationships in the concentration range of 0.05~100ng/g with good correlation coefficients(≥0.995).The limits of detection were 0.05~5.0ng/g(S/N=3)and the quantification were 0.15~15.0ng/g(S/N>10).The average recoveries were ranged from 76.4 % to117.7 % for 5 kinds of ginseng herbal medicines at 3 spiked levels.The relative standard deviations(RSD,n=3)were in the range of 0.54 % to 10.21 %.This method is sensitive,stable,simple and accurate,can solve the problem of matrix interference in the current detection standards of Traditional Chinese medicine.

关 键 词：超高效液相色谱-串联质谱法 QUECHERS 参类 中药材 农药残留 

分 类 号：TS207.3[轻工技术与工程—食品科学]