Full
Outline
To establish a method for the determination of nitroimidazole drugs residues in egg, chicken and pork matrices by high performance liquid chromatography-tandem mass spectrometry.
Samples were ultrasonically extracted with acetonitrile and acetonitrile-water solution, followed by degreasing with N-hexane saturated with acetonitrile. After centrifugation, the lower extract was purified using a Prime HLB solid-phase extraction column to instrumental analysis. Separation was achieved on a C18 column (2.1 mm×100 mm, 1.8 μm) with a gradient elution using 0.1% formic acid in water and acetonitrile as mobile phases. Quantification was performed by the external standard method.
The 10 kinds of nitroimidazole drugs exhibited good linearity within the range of 1–100 ng/mL, with correlation coefficients (r2) exceeding 0.995. The limit of quantitation for all compounds was 1.0 μg/kg. Average spike recoveries at 3 levels (1, 2 and 10 time limit of quantitation) ranged from 80.1% to 107.7%, with relative standard deviations between 0.8% and 7.5%. Analysis of 150 batches of samples using this method detected 3 positive batches: Metronidazole was identified in 2 egg samples (896.0 μg/kg and 1341.3 μg/kg), and dimetridazole was found in 1 chicken sample (480.2 μg/kg).
This method is highly efficient and accurate, capable of conducting qualitative and quantitative analysis of nitroimidazole drugs in pork, chicken and egg products. It effectively addresses the issues of incomplete food matrix and cumbersome operation in the current national standards, and provides technical support for ensuring the hygiene and safety of animal-derived foods.
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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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