Chinese Journal of Pharmaceutical Analysis >

2024 , Vol. 44 >Issue 7: 1169 - 1175

DOI: https://doi.org/10.16155/j.0254-1793.2023-0741

Ingredient Analysis

Determination of vitamin D3 in vitamin D drops by high resolution sampling two-dimensional chromatography*

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  • 1. Xiamen Institute for Food and Drug Quality Control, Xiamen 361012, China;
    2. Sinopharm Xingsha PharmaceuticalsXiamen Co., Ltd., Xiamen 361026, China

Received date: 2023-11-20

  Online published: 2024-08-05

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Abstract

Objective: To establish an innovative analytical method based on high resolution sampling two-dimensional chromatography (HiRes 2D-LC) for determination of the content of vitamin D3 in vitamin D drops. Methods: Two-dimensional liquid chromatography was used. Thermo HYPERSIL Gold Silica (100 mm×2.1 mm, 1.9 μm) column was used in the first dimension with n-hexane-n-amyl alcohol (996∶4) as mobile phase. The flow rate was 0.2 mL·min-1. The samples were injected and tested at the wavelength of 265 nm. The column temperature was 40 ℃. In the second dimension liquid chromatography, ShimPack Velox Hilic (50 mm×2.1 mm, 2.7 μm) was used as the column with n-hexane-n-pentanol-isopropanol (98∶1∶1) as the mobile phase. The flow rate was 0.5 mL·min-1. The samples were injected and tested at the wavelength of 265 nm. The column temperature was 40 ℃. A six-position 14-way valve and was equipped with 2 multi-center cutting valves was equipped to make multiple consecutive cuts of the pre-vitamin D3 peak and vitamin D3 peak. Results: The calibration curves showed a good linearity at the range of 1.018 4-5.092 mg·mL-1(r≥0.999 8). The precision test showed the RSDs of the peak area of pre-vitamin D3 and vitamin D3 were 0.95% and 0.40%, respectively. The repeatability test showed the RSD of vitamin D3 content was 0.41%. The average recovery rate (n=9) was 101.4%. The test solution was stable at 4 ℃ and 10 ℃ for 12 h, and the RSDs were 0.58% and 0.66%, respectively. The contents of vitamin D3 in the samples of vitamin D drops measured by this method were 100.4%, 101.6%, 100.9%, 101.6%, 102.7% and 101.6%, which was basically consistent with the results measured by the fourth method in General Chapter 0722 of ChP 2020 Vol Ⅳ. Conclusion: This method has a good specificity and high sensitivity to accurately determine the content of vitamin D3 in vitamin D drops.

Key words： high resolution sampling; two-dimensional chromatography; normal plase chromatography; vitamin D drops; pre-vitamin D3; vitamin D3; normal-phase chromatography; peak purity confirmation

Cite this article

WU Jue, GUO Wei-bin, QIU Xiao-feng, ZHENG Shu-feng . Determination of vitamin D3 in vitamin D drops by high resolution sampling two-dimensional chromatography*[J]. Chinese Journal of Pharmaceutical Analysis, 2024 , 44(7) : 1169 -1175 . DOI: 10.16155/j.0254-1793.2023-0741

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