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To identify the related substances in desloratadine using two-dimensional liquid chromatography-mass spectrometry (2D LC-MS) technology.
A Waters Symmetry C8 column (250 mm×4.6 mm, 5 μm) was employed. The mobile phase A consisted of a mixture containing 1% triethylamine and 10 mmol·L-1 potassium dihydrogen phosphate solution adjusted to pH 2.0 with phosphoric acid, acetonitrile, and methanol(80：10：10), while mobile phase B contained 1% triethylamine, 10 mmol·L-1 potassium dihydrogen phosphate solution(pH adjusted to 2.0 with phosphoric acid), acetonitrile, and tetrahydrofuran (30：70：5). A linear gradient elution was used for the first-dimension liquid chromatography separation of related substances in desloratadine. Individual separated components were captured through a multi-channel switching valve into retention vessels, then transferred to a Thermo BDS Hypersil C18 column (100 mm×4.6 mm, 3 μm). After a second-dimension gradient elution with a mobile phase composed of 10 mmol·L-1 ammonium acetate solution and methanol to achieve rapid desalting, electrospray ionization positive ionization-quadrupole-time-of-flight high-resolution mass spectrometry was employed to measure the accurate masses and elemental compositions of parent ions and their daughter ions of the related substances. Structural identification was achieved through spectral analysis.
Under the established analytical conditions, desloratadine and its related substances were well separated. A total of 12 related substances were detected and identified in desloratadine and its stressed degradation samples. Among these 12 degradants, three were known impurities, while the others are newly identified impurities.
2D LC-MS can effectively provide specific identification of desloratadine’s related substances under non-volatile mobile phase separation conditions. The findings from this study serve as a reference for controlling the quality of desloratadine.
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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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