Ingredient Analysis

Determination of enantiomeric purity D-Ala1-somatostatin in Somatostatin by HILIC HPLC*

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  • 1. SDU-ZB Biomedical Research & Development Institute, Zibo 255035, China;
    2. National Engineering and Technology Research Center of Chirality Pharmaceutical, Lunan Pharmaceutical Group Co., Ltd., Linyi 273400, China

Revised date: 2021-11-16

  Online published: 2024-06-26

Abstract

Objective: To establish an HILIC HPLC method for the determination of enantiomer impurity(D-Ala1-somatostatin, Alanine of position 1 has a D-type structure in SS)in somatostatin (SS). Methods: A Welch amino-column was used, with the mobile phase of phosphate buffer (0.02 mol·L-1 ammonium dihydrogen phosphate and 0.03 mol·L-1 tetrabutyl ammonium hydrogen sulfate aqueous solution, which previously adjusted to pH 3.0 with ammonia)-methanol-isopropanol (275∶362.5∶362.5) at the flow rate of 1.0 mL·min-1, at the detection wavelength of 215 nm. Results: It was linear for enantiomer impurity in the range of 1.022-10.22 μg·mL-1 (r=0.999 1). The average recovery of enantiomer impurity was 102.0%, with RSD of 1.5%. The detection limit of enantiomer impurity was 0.103 μg·mL-1, and the quantitation limit was 0.320 μg·mL-1. There was no enantiomer impurity in 7 samples. The enantiomer impurity was detected by high temperature and light during stability investigation. Conclusion: The method is accurate, reliable, reproducible, and suitable for the determination of enantiomer impurity, which provides a reliable method for quality control.

Cite this article

LIN Feng-Qiang . Determination of enantiomeric purity D-Ala1-somatostatin in Somatostatin by HILIC HPLC*[J]. Chinese Journal of Pharmaceutical Analysis, 2022 , 42(3) : 419 -423 . DOI: 10.16155/j.0254-1793.2022.03.08

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