目的 利用液相色谱-串联质谱(LC-MS/MS)和气相色谱-串联质谱(GC-MS/MS)检测技术建立人参中33种禁用农药多残留测定方法。方法 选取我国农业部明确在中草药种植中禁止使用的33种农药53个化学单体作为检测指标。以乙腈为溶剂,高速匀浆提取。检测方法:液相色谱-串联质谱法,采用十八烷基硅烷键合硅胶柱(2.1 mm×15 cm,1.6 μm)以0.1％甲酸(含5 mmol·L-1甲酸铵)溶液为流动相A,以95%乙腈溶液(含5 mmol·L-1甲酸铵、0.1％甲酸)为流动相B,离子源为电喷雾(ESI)离子源,正离子扫描模式下多反应监测(MRM)。气相色谱-串联质谱法,采用质量分数50%苯基甲基聚硅氧烷为固定液的弹性石英毛细管柱(30 m×0.25 mm,0.25 μm, DM17ms),以三重串联四极杆质谱仪检测,离子源为电子轰击源(EI),质谱监测模式为多反应监测(MRM)。结果 33种农药在2到20 ng·mL-1内各农药的相关系数r均大于0.990 0,呈良好的线性关系。做低水平及高水平回收(0.01和0.04 mg·kg-1),每个水平重复5次,结果平均回收率在87.57%~120.98%,RSD在1.45%~14.03%之间。结论 本方法能快速有效地检测人参中的农药多残留。
Abstract
OBJECTIVE To establish a method for the determination of 33 kinds of pesticide residues in Panax ginseng C.A.Mey by GC-MS/MS and LC-MS/MS. METHODS The 53 chemical monomers of 33 pesticide residues clearly prohibited by the Chinese ministry of agriculture were selected as the detection indicators. The samples were extracted with acetonitrile by high speed homogenizer. An LC-MS/MS analysis was performed on a CORTECSTM UPLC C18(2.1 mm×150 mm, 1.6 μm) column with isocratic elution of 0.1% formic acid (containing 5 mmol·L-1 ammonium formate) is mobile phase A, 95% acetonitrile(containing 5 mmol·L-1 ammonium formate and 0.1% formic acid)is mobile phase B.Electrospray ionization(ESI)source was applied by positive ionization in multiple reaction monitoring(MRM)modes. GC-MS/MS analysis was performed on a DM17ms(30 m×0.25 mm, 0.25 μm)capillary column with electron impact(EI)source, electron impact (EI) source was applied by positive ionization in multiple reaction monitoring modes (MRM). RESULTS The correlation coefficient r of 33 pesticide residues showed good linearity in the linear range of 2 to 20 ng·mL-1 was greater than 0.990 0. The average recoveries at spiked levels of low level and high level (0.01 and 0.04 mg·kg-1), repeat 5 times per level. The average recovery was 87.57%-120.98%, and the RSD was between 1.45%-14.03%. CONCLUSION The method can quickly and effectively detect pesticide residues in ginseng.
关键词
液相色谱-串联质谱 /
气相色谱-串联质谱 /
禁用农药 /
多残留分析 /
人参
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Key words
LC-MS/MS /
GC-MS/MS /
forbidden pesticide residues /
multi-residue analysis /
Panax ginseng C.A.Mey
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中图分类号：
R284
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参考文献
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脚注
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基金
国家十二五“重大新药创制”专项资助(2014ZX09304307-002);国家药典委员会药品医疗器械审评审批制度改革项目资助(ZG2016-2)
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