Full
Outline
To establish a method for the simultaneous deterction of chlorate and perchlorate in liquid milk by liquid chromatography-tandem mass spectrometry (LC-MS/MS).
Using liquid milk as the base, the contamination levels of chlorate and perchlorate were determined by LC-MS/MS. The instrument conditions, sample extraction and sample purification were tested and optimized, and the methodology of the optimized method was investigated.
The optimized detection method employed an ACQUITY UPLC®HSS T3 chromatographic column (2.1 mm×100 mm, 1.8 µm), with the mobile phase consisting of acetonitrile and 0.1% formic acid aqueous solution, at a flow rate of 0.1 mL/min and an injection volume of 5 µL. The extract from the sample was 2.0 mL of 0.1% formic acid aqueous solution and 8.0 mL of acetonitrile. The solid-phase extraction column was used the SelectCore HLB-V high chlorate-specific column (150 mg/3 mL). The internal standard method was used for quantitative detection of chlorate and perchlorate in liquid milk. The linear relationship of chlorate and perchlorate in their respective linear ranges was good. The determination coefficient of chlorate was 0.9995, and that of perchloric acid salt was 0.9998. The limit of detection chlorate was 2.4 µg/kg and that of perchlorate was 0.8 µg/kg. The recovery rate of actual sample detection with spiked samples was between 81.9% and 105.4%. The relative standard deviation (RSD) was less than to 10%, meeting the requirements for quantitative detection.
This method has the characteristics of simple operation, high sensitivity, accurate quantification and good repeatability. It is suitable for the simultaneous detection of chlorate and perchlorate in complex liquid milk matrices.
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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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