To establish a method for simultaneous detection of 38 kinds of veterinary drug residues(including tetracyclines, sulfonamides, quinolones, β-agonists, amantadine, chloramphenicol, thiamphenicol, etc.) in raw pork puree for infant complementary foods by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS).
Samples were extracted with acetonitrile and ethylenediaminetetraacetic acid disodium salt (Na2EDTA)–Mcllvaine buffer, cleaned-up on an Oasis PRiME HLB cartridge, concentrated to dryness under nitrogen at 40 °C and reconstituted in 0.2% formic acid. Chromatographic separation was performed on a Phenomenex Kinetex® 2.6 µm EVO C18 column, and the analysis was conducted using multiple reaction monitoring with dynamic polarity switching via an Agilent Jet Stream electrospray ionization source (AJS ESI), with quantification based on a matrix-matched calibration standard approach.
The 10 kinds of target compounds and 28 kinds of target compounds showed good linear responses in the concentration ranges of 10–400 µg/L and 10–500 µg/L, respectively, and the correlation coefficients (r) of the obtained calibration curves were all no less than 0.995. The limits of detection were determined to range from 0.03 to 1.47 µg/kg, with the limits of quantitation established between 0.10 and 4.90 µg/kg. At 3 spiked levels of 5, 10 and 20 µg/kg (n=6), the average recoveries ranged from 64.32% to 111.66% with relative standard deviations of 2.17%–10.70%, meeting the requirements specified in GB/T 27404—2008 Specifications for quality control in laboratories-Physical and chemical testing of food.
This method offers straightforward operation, high sensitivity, good accuracy and precision,enabling high-throughput screening and confirmation of 38 kinds of veterinary drug residues in pork puree used as raw material for infant complementary foods.
| 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 |