Objective To establish a method for the determination of 2-hexylpyridine content in the milk and dairy product by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The sample was extracted by acetonitrile vortex extraction, and the analytical solution was purified by QuEChERS dSPE EMR Lipid degreasing tube. After centrifugation, it was tested on a membrane machine. The acetonitrile primary water as the mobile phase was used, the flow rate was set at 0.25 mL/min, the gradient elution procedure was applied, the GL Sciences InertSustain C18 chromatographic column was used for separation, the electro spray positive ion (ESI+) mode, the multiple reaction monitoring (MRM) mode was used for detection, and the matrix matching external standard method was used for quantification. Results The methodological validation indicators were well that the calibration curves were linear in the range of 0.5-20.0 ng/mL with the correlation coefficients (r2) larger than 0.998. The average recoveries of 2-hexylpyridine were 94.45%-109.63% and the relative standard deviations were 3.93%-9.53% at 0.005, 0.010 and 0.050 mg/kg with 3 kinds of spiked levels. Conclusion The accuracy, precision, and sensitivity of the method meet the requirements for residue detection.
| 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 |