Determination of 69 Kinds of Pesticide Residues in Paeonia tactilora ,Astragalus membranaceus ,Ranunculus ternatus and Cornus officinalis by GC-MS/MS
- VernacularTitle: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
- Author:
Qian WANG
1
;
Yanchun ZHU
1
;
Tingting LI
1
;
Leilei FAN
1
;
Zhenguo LI
1
;
Xueqin WANG
1
Author Information
1. Henan Provincial Institute for Food and Drug Control,Zhengzhou 450003,China
- Publication Type:Journal Article
- Keywords:
GC-MS/MS;
Paeonia tactilora;
Astragalus membranaceus;
Ranunculus ternatus;
Cornus officinalis;
Pesticide residues
- From:
China Pharmacy
2019;30(20):2829-2834
- CountryChina
- Language:Chinese
-
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.