Objective To establish a method for the rapid determination of 45 kinds of pesticides residues in Vitis vinifera by gas chromatography-tandem mass spectrometry (GC-MS/MS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods The Vitis vinifera samples were first extracted with acetonitrile by vibration and ultra-sonic. Then the mix adsorbents were used in dispersive solid phase extraction to purify the extract. After high speed centrifugation and filtration, the samples were detected by GC-MS/MS using selected reaction monitoring (SRM) mode, and LC-MS/MS using multiple reaction monitoring (MRM) mode. Results Deltamethrin exhibited good linearity within the concentration range of 0.1 to 1.0 mg/kg, while captan showed linearity within the range of 0.2 to 3.0 mg/kg, 28 kinds of pesticides including metalaxyl showed good linear relationships within the concentration range of 0.04-1.00 mg/kg, and 15 kinds of pesticides including emamectin benzoate showed good linear relationships within the concentration range of 0.1-1.0 mg/kg, with correlation coefficients reached 0.99 or above. The limits of detection were in the range of 0.00020-0.05000 mg/kg, the limits of quantitation were in the range of 0.00050-0.15000 mg/kg. The spiked recoveries at 3 levels of 45 kinds of pesticides were in range of 70.3%-117.0%, the relative standard deviations were in range of 0.01%-14.30%. Conclusion With features such as accuracy and easy operation, this method can be used to fast determination of 45 kinds of pesticides in Vitis vinifera without any special samples pretreatment apparatus, and also satisfies the requirement of pesticide routine analysis.
| 科 Family | 属数 Number of genus | 种数 Number of species | 占总种数比例 Percentage of total species (%) | 属 Genus | 种数 Number of species | 占总种数比例 Percentage of total species (%) |
|---|---|---|---|---|---|---|
| 鹅膏菌科Amanitaceae | 2 | 11 | 5.26 | 鹅膏菌属 Amanita | 10 | 4.78 |
| 小菇科 Mycenaceae | 2 | 12 | 5.74 | 丝盖伞属 Inocybe | 5 | 2.39 |
| 多孔菌科 Polyporaceae | 8 | 14 | 6.70 | 蜡蘑属 Laccaria | 5 | 2.39 |
| 红菇科 Russulaceae | 3 | 23 | 11.00 | 小皮伞属 Marasmius | 6 | 2.87 |
| 小菇属 Mycena | 11 | 5.26 | ||||
| 光柄菇属 Pluteus | 5 | 2.39 | ||||
| 红菇属 Russula | 17 | 8.13 | ||||
| 栓菌属 Trametes | 5 | 2.39 |