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Determination of Defibrase in Pharmaceutical Formulation by LC with 6-Aminoquinolyl-N-hydroxysuccinimidyl Carbamate Derivatization and Fluorescence Detection

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Abstract

A sensitive LC method with pre-column fluorescence derivatization using 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate has been developed for the determination of defibrase from the venom of Agkistrodon acutus (also named defibrase in the Chinese Pharmacopoeia) in pharmaceutical formulation. By a denaturing procedure prior to derivatization, full and homogeneously derivatization of defibrase was obtained and demonstrated using MALDI-TOF-MS. The specificity of the method was validated by assessing interference from the placebo and by forced degradation. The method has demonstrated good linearity (r = 0.9998), accuracy (mean recovery 98.53%) and precision (RSD < 2.5%). Moreover, the method was found to be sensitive with a low limit of detection (3.35 ng mL−1) and limit of quantitation (10.16 ng mL−1). The method was successfully applied to the quantitative determination of defibrase in pharmaceutical formulation.

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Acknowledgments

The authors wish to thank MOST (The ministry of Science and Technology of the People’s Republic of China) for the financial support.

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Authors and Affiliations

  1. School of Pharmacy, Chinese Pharmaceutical University, 210009, Nanjing, Jiangsu, China

    Xiao-Qing Luo

  2. National Institute for the Control of Pharmaceutical and Biological Products (NICPBP), 100050, Beijing, China

    Hua-Xin Yang, Cheng-Gang Liang & Shao-Hong Jin

  3. Department of Pharmacy, Suzhou Health College, 215009, Suzhou, Jiangsu, China

    Xiao-Qing Luo

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  1. Xiao-Qing Luo
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  2. Hua-Xin Yang
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  3. Cheng-Gang Liang
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  4. Shao-Hong Jin
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Correspondence to Shao-Hong Jin.

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Luo, XQ., Yang, HX., Liang, CG. et al. Determination of Defibrase in Pharmaceutical Formulation by LC with 6-Aminoquinolyl-N-hydroxysuccinimidyl Carbamate Derivatization and Fluorescence Detection. Chroma 70, 1239–1244 (2009). https://doi.org/10.1365/s10337-009-1297-3

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