Objective To establish a non-derivatized extraction method for the simultaneous determination of chlorthal-diacid, dalapon and trysben in tea by liquid chromatography-tandem mass spectrometry (LC-MS/MS) combined with hydrophile-lipophile balance (HLB) clean-up. Methods Tea samples were extracted by 20 mL of 1% acetic acid in water and 10 mL of methylene chloride; clean-up by HLB (300 mg/3 mL) filtration. Separation of the target analytes was achieved on an octadecylsilane (C18) chromatographic column, and quantitation was performed by LC-MS/MS in negative ion mode. Results The 3 kinds of herbicides were effectively separated on the C18 column with good linearity in the range of 0.01-2.00 μg/mL (r2>0.997). At 4 spiked levels of 0.05, 0.25, 0.50 and 1.00 mg/kg, the average recoveries of the 3 kinds of pesticides in the blank matrix of tea ranged from 71.1% to 119.2%, with the relative standard deviations between 3.3% and 18.3%. The limits of detection were ranged from 0.002-0.009 mg/kg, and the limits of quantitation were ranged from 0.008-0.029 mg/kg of the 3 kinds of herbicides. Conclusion The developed method offers a simple and rapid pretreatment procedure, eliminating the need for derivatization. It is friendly to the inspectors and the environment, and can be used as a method for large-scale detection of chlorthal-diacid, dalapon and trysben residues in tea.
| 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 |