To establish a method for simultaneous determination of 6 kinds of pesticide residues in Polygonatum kingianum Coll. et Hemsl. by QuEChERS-high performance liquid chromatography-tandem mass spectrometry.
The pulverized Polygonatum kingianum Coll. et Hemsl. samples were homogeneously extracted with ethyl acetate-acetonitrile solution (1:99, V:V). Magnesium sulfate anhydrous, primary secondary amine and octadecylsilane bonded silica gel sorbents were used for purification. The 6 kinds of pesticide residues in Polygonatum kingianum Coll. et Hemsl. were analyzed by high performance liquid chromatography-tandem mass spectrometry under positive electrospray ionization mode, and quantified via matrix-matched external standard method.
The 6 kinds of pesticides exhibited good linear relationships within the mass concentration range of 2–100 ng/mL,with all coefficients of determination greater than 0.995. The limits of detection were 0.07–0.46 μg/kg, and the limits of quantitation were 0.14–0.91 μg/kg. At 3 spiked concentration levels, the overall average recoveries of the 6 kinds of pesticides ranged from 90.4% to 100.7%, and the relative standard deviations (n=6) were 0.8%–2.3% (all less than 15%).
This method is rapid, efficient, accurate with favorable precision and sensitivity. It can meet the requirements for quantitative analysis of the 6 kinds of pesticide residues in Polygonatum kingianum Coll. et Hemsl.,and provides fundamental technical support for monitoring the edible quality safety and medicinal quality consistency of Polygonatum kingianum Coll. et Hemsl.
| 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 |