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To establish a solid-phase extraction-high performance liquid chromatography(SPE-HPLC) method for the rapid detection of related substances of vitamin D3, trans vitamin D3 (impurity A), 7-dehydrocholesterol (impurity B), lumisterol 3 (impurity C), and isotachysterol 3 (impurity D), in vitamin D drops (soft capsules).
The content, which was approximately equivalent to vitamin D3 1 548 IU, was taken in about 1.2 g, weighed accurately, put into a test tube, 4 mL of isooctane was added to it, and it was swirled and mixed well. Purification was performed using solid phase extraction columns, with n-hexane-ethyl acetate(85∶15) as the elution agent and anhydrous ethanol as the desorption agent. A Luna Silica(2) 100 Å silica gel column(150 mm×4.6 mm, 3 μm) was used, with n-hexane-n-pentanol (996.5∶3.5) as the mobile phase. The content of vitamin D3 impurities was calculated using the adding standard calibration factors principal component self-control method.
The separation degree between pre-vitamin D3 and vegetable oil was greater than 1.5. The linear range of vitamin D3 was 0.02-0.80 μg·mL-1, with r=0.999 5. The linear range of impurity A was 0.02 -0.80 μg·mL-1, with r=0.999 9. The linear range of impurity B was 0.02-0.80 μg·mL-1, with r=0.999 9. The linear range of impurity C was 0.02-0.80 μg·mL-1, with r=0.999 9. The linear range of impurity D was 0.02-0.80 μg·mL-1, with r=0.999 9. The average recovery rate of impurities A-D (n=9) was 93.2%-102.9%. The detection results of 3 batches of vitamin D drops (soft capsules) showed that the content of known impurities and other maximum single impurities were less than 0.5%, and the total content of impurities was less than 1.0%.
The results indicate that the established method is suitable for the detection of vitamin D3 related substances in vitamin D drops (soft capsules). It has the advantages of being easy to operate, providing rapid and accurate results, and providing technical assurance for the quality control of fat-soluble vitamin D3 preparations.
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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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