Determination of 69 Kinds of Pesticide Residues in Paeonia tactilora ，Astragalus membranaceus ，Ranunculus ternatus and Cornus officinalis by GC-MS/MS / 中国药房

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.