Full
Outline
To establish a method for determination of 48 kinds of pesticide and veterinary drug residues in crayfish by pass-through purification coupled with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS).
The samples were first extracted using a 80% acetonitrile solution, and then cleaned-up by hydrophilic-lipophilic column in a pass-through mode and filtered through a filter, then separated employing an C18 column. The mass spectrometer operated with electrospray ionization in multiple reaction monitoring mode and quantified by matrix-matched external standard curve method.
The results demonstrated that all the analytes had satisfactory linearity in the range of 1–100 ng/mL with correlation coefficients (r) greater than 0.997. The limits of detection and the limits of quantitation were in the ranges of 0.02–0.20 and 0.05–0.50 μg/kg, respectively. The average recoveries at 3 spiked levels with 6 parallel determinations ranged between 70.2%–105.8%, with the relative standard deviations no more than 3.3%, which met the requirements of trace analysis. The 36 samples from major producing areas were analyzed, revealing a drug detection rate of 20.8%. The positive results showed high consistency when retested against standard methods.
This method is simple, rapid, sensitive and accurate, effectively reducing matrix interference from the complex composition of crayfish. It satisfies the screening requirements for pesticide and veterinary drug residues in crayfish under the rice-crayfish integrated farming model, providing a crucial technical tool for quality safety control and risk assessment.
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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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