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Sensitive Quantitation of Residual Phenylhydrazine in Antipyrine by LC-ICP-MS with Iodo Derivatization

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Abstract

Phenylhydrazine is a genotoxic impurity commonly used as a raw material in active pharmaceutical ingredients. In this study, a novel method, using inductively coupled plasma-mass spectrometry combined with two-dimensional liquid chromatography (LC-ICP-MS), was employed for the quantitation of residual phenylhydrazine in antipyrine. The compound 2,3,5-triiodobenzoyl chloride, which contains three iodine atoms, was investigated as a derivatization reagent. The DL 0.06 ppm was obtained, and the method was applied to the quantitation of residual phenylhydrazine in antipyrine. No residual phenylhydrazine was detected in five lots of antipyrine obtained from the commercial source.

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Author notes

  1. Koki Harigaya

    Present address: Technology Department, Yoshitomi Plant, Mitsubishi Tanabe Pharma Factory Ltd., 955 Koiwai, 871-8550, Yoshitomi, Chikujo, Fukuoka, Japan

Authors and Affiliations

  1. Analytical Research Laboratories, CMC Division, Mitsubishi Tanabe Pharma Corp, 3-16-89 Kashima, 532-8505, Yodogawa, Osaka, Japan

    Koki Harigaya, Hiroyuki Yamada & Shingo Horimoto

  2. Department of Pharmaceutical Chemistry, Faculty of Pharmacy, Yasuda Women’s University, 6-13-1 Yasuhigashi, 731-0153, Asaminami, Hiroshima, Japan

    Hiroyuki Nishi

  3. School of Pharmacy and Pharmaceutical Sciences, Mukogawa Women’s University, 11-68 Koshien Kyuban-cho, 663-8179, Nishinomiya, Japan

    Jun Haginaka

Authors
  1. Koki Harigaya
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  2. Hiroyuki Yamada
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  3. Shingo Horimoto
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  4. Hiroyuki Nishi
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  5. Jun Haginaka
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Correspondence to Koki Harigaya.

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Harigaya, K., Yamada, H., Horimoto, S. et al. Sensitive Quantitation of Residual Phenylhydrazine in Antipyrine by LC-ICP-MS with Iodo Derivatization. ANAL. SCI. 30, 845–850 (2014). https://doi.org/10.2116/analsci.30.845

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  • DOI: https://doi.org/10.2116/analsci.30.845

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