Full
Outline
To establish a method for the simultaneous determination of 9 kinds of sweeteners(neotame, aspartame, alitame, aspartame, sodium cyclamate, acesulfame potassium, saccharin sodium, sucralose and stevioside) in chocolate by high performance liquid chromatography-quadrupole/electrostatic field orbital hydrazine high resolution mass spectrometry.
The chocolate samples were hydrolyzed with 1 mol/L hydrochloric acid at 60 ℃ for 1 h, then passed through an HLB solid-phase extraction column. The eluate was nitrogen-blown, and the residue was dissolved in water and made up to 1.0 mL. After thorough vortex mixing, it was filtered through a 0.45 μm filter membrane. Separation was performed on a Phenomenex C18 (100 mm×4.6 mm, 2.6 μm) chromatographic column using a gradient elution program with acetonitrile-water solution as the mobile phase. Mass spectrometry was conducted in negative ion mode, with a scanning range of 100–1000 m/z. The secondary scan mode was fullMS-ddMS, and quantification was carried out by the external standard method.
Under the established chromatographic conditions, 9 kinds of sweeteners could be well separated. The limits of detection for the 9 kinds of sweeteners were 7.0 μg/kg, and the limits of quantitation were 20.0 μg/kg. The linear relationship was good within the concentration range of 20–200 ng/mL, and the correlation coefficients were all greater than 0.99. Through spiked verification, the average recovery range of the 3 levels was in the range of 75.3%–110.2%, with a relative standard deviations in the range of 3.2%–8.9%.
This method is efficiency and rapid for sample pretreatment. It can be used for high-throughput determination of 9 kinds of sweeteners in chocolate. The established method provides a reliable and accurate technical means for trace detection of sweeteners in food, and is of great significance for regulating the use of food additives in food.
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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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