Full
Outline
To establish a method for the rapid determination of 6 kinds of biogenic amines in fermented milk by pass-through solid-phase extraction coupled with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS).
After extraction with a 2% formic acid/acetonitrile solution, samples were purified using an Oasis PRiME HLB solid-phase extraction cartridge to efficiently remove interferences such as proteins and phospholipids. Chromatographic separation was performed on a hydrophilic interaction chromatography column. Mass spectrometric detection was carried out in multiple reaction monitoring mode, and quantification was achieved by the internal standard method.
The method was validated and demonstrated good linearity (r2≥0.996)for the 6 kinds of biogenic amines within a certain concentration range, the limits of detection were 0.20 µg/kg–1.80 µg/kg,the limits of quantitation were 0.67–6.00 µg/kg. Spiked recoveries were 76.0%–117.8%, with relative standard deviations below 13%. Analysis of commercial fermented dairy samples revealed that tyramine was the predominant biogenic amine, with concentrations ranging from 0.80 to 1.70 mg/kg, while safety-risk-associated biogenic amines such as histamine were detected at extremely low levels or were not detected.
The established method,by incorporating the Oasis PRiME HLB purification strategy, effectively resolves the critical issue of phospholipid interference in dairy products. It features advantages such as simple and rapid sample preparation, high sensitivity and strong anti-interference capability. The method is suitable for the high-throughput determination of multiple biogenic amines in fermented dairy products, providing robust technical support for the quality control and safety risk assessment of these products.
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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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