Objective: To establish a simple and rapid method to determine the content of vitamin D3 in vitamin D/AD drops (soft capsules). Methods: The appropriate amount of the content of the preparation was directly diluted with n-hexane to a suitable concentration for high performance liquid chromatography-tandem triple quadrupole mass spectrometry (LC-QQQ) detection.The chromatographic columnwas Agilent Zorbax Rx-Sil (100 mm×3.0 mm, 1.8 μm). The mobile phase was n-hexane-n-pentane alcohol(997∶3). Flow rate: 1 mL·min-1, column temperature:35 ℃, APCI source, MRM mode, m/z 385.3→259.1 (+) (quantitative ion). 0-5 min to waste, and then after 5min to mass. Results: The pre-vitamin D3 and vitamin D3 had the same response factor in the mass spectrometry detection, and their peak area could be directly combined to calculate the content; the linear range of total vitamin D3 was 0.01-0.5 μg·mL-1(r=0.999 5); the average recoveries (n=9) of vitamin D3 in the four vitamin D/AD drops (soft capsules) samples were between 100.5% and 102.3%. Multi-batch of the four vitamin D/AD drops (soft capsules)were detected, and the vitamin D3 in the preparation samples were within the validity period reached 90.0%-105.0% of the labeled amount. Conclusion: This method has been validated by methodology and is suitable for the determination of vitamin D3 content in vitamin D/AD drops (soft capsules) without any pre-treatment steps or determination of the relative correction factor of the precholecalciferol.The operation is simple, fast and accurate, and provides a reference for the content detection of other oil-soluble vitamin D3 preparations.
ZHOU Jing-ming, XU Fu-chun, CHEN Xiu-ming, SHI Zhen-xiang, LIN Bin, CHEN Xi-sheng, SU Zhi-wei, FANG Dong-sheng
. Determination of vitamin D3 in vitamin D/AD drops (soft capsules) by high performance liquid chromatography-tandem triple quadrupole mass spectrometry[J]. Chinese Journal of Pharmaceutical Analysis, 2022
, 42(5)
: 780
-788
.
DOI: 10.16155/j.0254-1793.2022.05.05
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