Full
Outline
To establish a method for the quantitative determination of 13 kinds of pesticide residues, including chlorothalonil, chlorpropham and diquat, in palm oil by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).
Palm oil samples were extracted with acetonitrile in a citric acid system. This method employed octadecylsilane-bonded silica gel (C18) for defatting purification. This study employed liquid chromatography-tandem mass spectrometry for detection, with external standard quantification. Using a 5 mmol/L ammonium acetate aqueous solution-methanol mixture as the mobile phase, perform gradient elution. Chromatographic separation was performed using a Kinetex C18 column (100 mm×4.6 mm, 2.6 μm), multi-reaction monitoring mode. The electrospray ionization source (ESI) simultaneously scaned the positive ion mode and negative ions.
In 2 kinds of food matrices—palm oil and palm kernel oil, 13 kinds of pesticides exhibited good linear relationships within their respective concentration ranges and the correlation coefficient was greater than 0.990. The limit of detection was 0.003 mg/kg, and the limit of quantitation was 0.01 mg/kg. Method validation experiments were conducted on palm oil and palm kernel oil at 3 different spiked levels. The results showed that the recovery rates of 13 kinds of pesticides on the 2 kinds of substrates ranged from 71.0% to 112% and 80.1% to 108.5%, respectively. With relative standard deviations all below 15%. The intraday precision ranges for palm oil and palm kernel oil were 1.0%–9.3% and 1.6%–8.8%, and the daytime precision ranges were 2.9%–15.6% and 2.6%–9.3%, respectively.
This method features simple pretreatment, high sensitivity, and good accuracy, making it suitable for the qualitative screening and precise quantitative analysis of 13 kinds of pesticide residues in palm oil. It provides a testing basis for food imports and exports.
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| 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 |
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