Determination of 4-hydrazine benzoic acid content in deferasirox by acetone solution derivatization-HPLC

doi:10.16155/j.0254-1793.2021.12.08

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Chinese Journal of Pharmaceutical Analysis ›› 2021, Vol. 41 ›› Issue (12) : 2102-2106. DOI: 10.16155/j.0254-1793.2021.12.08

Safety Monitoring

Determination of 4-hydrazine benzoic acid content in deferasirox by acetone solution derivatization-HPLC

YU Xiao-yan, XIE Chun-wen^*, WU Xiao-dong, WANG Hong-jie, SHA Sha, LI Liang-Liang, CAO Huan-ying

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Abstract

Objective: To develop a method for determination of 4-hydrazine benzoic acid content in deferasirox by acetone solution derivatization-HPLC. Methods: 4-hydrazine benzoic acid was derivatized by acetone solution [phosphoric acid-acetone-water(25∶100∶900)].The analysis was carried out on a Symmetry Shield C₁₈(150 mm×4.6 mm,3.5 μm)column, mobile phase A: phosphoric acid-acetonitrile-water (2∶100∶900),mobile phase B: phosphoric acid-water-acetone (2∶100∶900). The flow rate was 1.0 mL·min^-1 in a gradient mode. The detection wavelength was 316 nm. The column temperature was set at 40 ℃ and the injection volume was 25 μL. Results: The limit of quantitation was 15.5 ng·mL^-1. The limit of detection was 7.7 ng·mL^-1. The linear range was 15.7-785.7 ng·mL^-1(r²=0.999 7). Average recoveries were 95.2%(RSD=4.8%, n=9). The RSD for repeatability of six samples was 4.8%.The RSD for intermediate precision of twelve samples was 4.4%. When the chromatographic conditions were changed slightly, The RSD of 4-hydrazine benzoic acid content was 3.8%. Conclusions: The established method has high accuracy and specificity. It can be used for quality control of deferasirox crude drug.

Key words

4-hydrazine benzoic acid / deferasirox / acetone / derivatization / HPLC

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YU Xiao-yan, XIE Chun-wen, WU Xiao-dong, WANG Hong-jie, SHA Sha, LI Liang-Liang, CAO Huan-ying. Determination of 4-hydrazine benzoic acid content in deferasirox by acetone solution derivatization-HPLC[J]. Chinese Journal of Pharmaceutical Analysis, 2021, 41(12): 2102-2106 https://doi.org/10.16155/j.0254-1793.2021.12.08

References

[1] CHANNON RB, NEWLAND JC, BRISTOW AWT, et al. SeLective detection of hydrazine in the presence of excess eLectrochemicaLLy active pharmaceuticaL ingredients using boron doped diamond metaL nanoparticLe functionaLised eLectrodes [J].Electroanalysis, 2013, 25(12): 2613
[2] REDDY AVB, JAAFAR J, UMAR K, et al. Identification, control strategies, and analytical approaches for the determination of potential genotoxic impurities in pharmaceuticals: a comprehensive review [J].J Sep Sci, 2015, 38(5): 764
[3] 刘爱赟,袁永兵,靳文仙,等. 药物中肼类基因毒性杂质分析研究进展[J].药物评价研究,2020,43(2):356
LIU AB, YUAN YB, JIN WX,et al.The development of hydrazide genotoxic impurity[J].Drug Eval Res, 2020,43(2):356
[4] MUNRO IC, RENWICK AG, DANIELEWSKA-NIKIEI B. The threshold of toxicologicaL concern (TTC) in risk assessment [J].Toxicol Lett, 2008, 180(2): 151
[5] CHANNON RB, JOSEPH MB, BITZIOU E, et al. ELectrochemical flow injection analysis of hydrazine in an excess of an active pharmaceutical ingredient: achieving pharmaceutical detection limits electrochemically [J].Anal Chem, 2015, 87(19): 10064
[6] 阮晓玲,郑项元,徐洁,等. 药物中基因毒性杂质分析方法的研究进展[J].中国药科大学学报,2016,47(3):267
RUAN XL, ZHENG XY, XU J, et al. The development of genotoxic impurity in drug [J].J China Pharm Univ,2016,47(3):267
[7] LAKSHMI KJ, DEVI PR, MUKKANTI K. Quantitative determination of residual hydrazine content in cilazapril by ion chromatography [J].Orient J Chem, 2010, 2(3): 1001
[8] REDDY VB, VENUGOPAL N, MADHAVI G. A selective and sensitive LC-MS/MS method for the simultaneous determination of two potential genotoxic impurities in celecoxib[J].J Anal Sci Technol, 2014, 5(1): 1
[9] KEAN T, MILLER JH, SKELLERN GG, et al. Acceptance criteria for levels of hydrazine in substances for pharmaceutical use and analytical methods for its determination[J].Pharm Sci Notes, 2006(2): 23
[10] SUN M, BAI L, TERFLOTH GJ, et al. Matrix deactivation: a generaL approach to improve stability of unstable and reactive pharmaceutical genotoxic impurities for trace analysis[J].J Pharm Biomed Anal, 2010, 52(1):30
[11] OH JA, PARK JH, SHIN HS. Sensitive determination of hydrazine in water by gas chromatography-mass spectrometry after derivatization with ortho-phthalaldehyde[J].Anal Chim Acta, 2013, 769 (6):79
[12] OH JA, SHIN HS. Simple and sensitive determination of hydrazine in drinking water byultra-high-performanceliquid chromatography-tandem mass spectrometry after derivatization with naphthalene-2, 3-dialdehyde[J]. J Chromatogr A, 2015, 1395: 73