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GC-MS/MS法同时测定白芍、黄芪、猫爪草和山茱萸中69种农药的残留量
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| 篇名： | GC-MS/MS法同时测定白芍、黄芪、猫爪草和山茱萸中69种农药的残留量 |
| TITLE： | |
| 摘要： | 目的：建立同时测定白芍、黄芪、猫爪草和山茱萸中69种农药残留量的方法。方法：采用气相色谱-串联质谱法。色谱柱为HP-5MS弹性石英毛细管柱，进样口温度为240 ℃，进样量为1 μL，不分流进样，载气为高纯氦气，进样口模式为恒压模式，柱前压力为146 kPa，程序升温；质谱仪为三重四级杆串联质谱仪，离子源为电子轰击源，离子源温度为230 ℃，离子化能量为70 eV，碰撞气为氮气，质谱传输接口温度为280 ℃，四级杆温度为150 ℃，监测模式为多反应监测（MRM），溶剂延迟时间为5 min。结果：69种农药残留的检测质量浓度线性范围为4.82～399.6 ng/mL（r均大于0.990）；定量限为0.001 7～0.013 3 mg/kg，检出限为0.000 5～0.004 mg/kg；精密度、稳定性试验的RSD均小于10％（n＝6），重复性试验的RSD均小于5％（n＝6；仅检出杀虫脒、氯菊酯）；加样回收率为62.9％～123.5％（RSD均小于10％，n＝6）。12批样品中，山茱萸中检出敌敌畏、二苯胺，黄芪中检出杀虫脒、氯菊酯，白芍中检出二苯胺、杀虫脒，猫爪草中检出二苯胺、乙烯菌核利，其他成分均未检出。结论：该方法操作简便、重复性好，可用于同时测定白芍、黄芪、猫爪草和山茱萸中69种农药的残留量。 |
| ABSTRACT： | OBJECTIVE： To establish the method for simultaneous determination of 69 kinds of pesticide residues in Paeonia tactilora， Astragalus membranaceus， Ranunculus ternatus and Cornus officinalis. METHODS： GC-MS/MS method was adopted. The determination was performed on HP-5MS fused silica capillary column with splitless injecting samples. The injector temperature was set at 240 ℃， and sample size was 1 μL. The carrier gas was high-purity helium， the inlet mode was constant pressure， the pre-column pressure was 146 kPa， and the temperature was programmed. Triple four-pole tandem mass spectrometry was used for the detection， and electron impact ion source was used as ion source. The temperature of the ion source was 230 ℃， ionization energy was 70 eV， and the collision gas was nitrogen. The inlet temperature was 280 ℃ and four-pole temperature was 150 ℃， mass spectrometry monitoring mode was multi-reaction monitoring （MRM）， and solvent delay time was 5 min. RESULTS： The linear range of 69 kinds of pesticide residue was 4.82-399.6 ng/mL （all r＞0.990）. LODs were all in the range of 0.001 7-0.013 3 mg/kg， and LOQs were all in the range of 0.000 5-0.004 mg/kg. RSDs of precision and stability tests were less than 10％ （n＝6）. RSD of reproducibility test was lower than 5％ （n＝6， only pesticide amidine and permethrin were detected）. The recoveries were in the range of 62.9％-123.5％ （all RSD＜10％， n＝6）. Among 12 batches of samples， dichlorvos and diphenylamine were detected in C. officinalis； chlordimeform and permethrin were detected in A. membranaceus； diphenylamine and chlordimeform were detected in P. tactilora； diphenylamine and vinclozolin were detected in R. ternatus. CONCLUSIONS： The method is simple in operation and reproducible for simultaneous determination of 69 kinds of pesticide residue in P. tactilora， A. membranaceus， R. ternatus and C. officinalis. |
| 期刊： | 2019年第30卷第20期 |
| 作者： | 王倩，朱艳春，李婷婷，樊磊磊，李振国，王雪芹 |
| AUTHORS： | WANG Qian，ZHU Yanchun，LI Tingting，FAN Leilei，LI Zhenguo，WANG Xueqin |
| 关键字： | 气相色谱-串联质谱法；白芍；黄芪；猫爪草；山茱萸；农药残留量 |
| KEYWORDS： | GC-MS/MS； Paeonia tactilora； Astragalus membranaceus； Ranunculus ternatus； Cornus officinalis； Pesticide residues |
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