Identification of unknown impurities in triamcinolone acetonide palmitate

doi:10.5246/jcps.2022.04.024

Journal of Chinese Pharmaceutical Sciences ›› 2022, Vol. 31 ›› Issue (4): 270-278.DOI: 10.5246/jcps.2022.04.024

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Identification of unknown impurities in triamcinolone acetonide palmitate

Xiangfei Jin¹, Minyue Cheng¹, Sihui Zhong¹, Yungen Xu², Weiyang Shen¹^,³^,^*()

1 Department of Analytical Chemistry, China Pharmaceutical University, Nanjing 211198, China
2 Jiangsu Key Laboratory of Drug Design and Optimization, Department of Medicinal Chemistry, China Pharmaceutical University, Nanjing 211198, China
3 Key Laboratory of Drug Quality Control and Pharmacovigilance, Ministry of Education, Nanjing 210009, China

Received:2021-11-25 Revised:2021-12-08 Accepted:2021-12-15 Online:2022-04-30 Published:2022-04-30
Contact: Weiyang Shen

Abstract

Abstract:

In the present study, we analyzed the structures of the two unknown impurities that were contained more than 0.1% in triamcinolone acetonide palmitate by using HPLC-DAD and HPLC-MS hyphenated techniques, and these impurities were synthesized and purified by column chromatography. Based on the results of NMR spectroscopy, IR spectroscopy, and MS, the two impurities were confirmed as 9-fluoro-11β,21-dihydroxy-16α,17-(isopropylidenedioxy)pregna-1,4-diene-3,20-dione 21-myristate and stearate, respectively.

Key words: Triamcinolone acetonide palmitate, Impurity identification, HPLC-DAD, LC-MS

Supporting:

Xiangfei Jin, Minyue Cheng, Sihui Zhong, Yungen Xu, Weiyang Shen. Identification of unknown impurities in triamcinolone acetonide palmitate[J]. Journal of Chinese Pharmaceutical Sciences, 2022, 31(4): 270-278.

Figures/Tables 10

Table 1. Results of related substances of triamcinolone acetonide palmitate.

Table 2. Results of IR spectra of triamcinolone acetonide myristate and triamcinolone acetonide stearate.

Table 3. Results of 1H NMR spectra of triamcinolone acetonide myristate and triamcinolone acetonide stearate.

[1]	The United States Pharmacopeial Convention. Triamcinolone Acetonide, USP40–NF35. Rockville, MD. 2015, 6558–6559.
[2]	The United States Pharmacopeial Convention. Cetyl Palmitate, USP40–NF35. Rockville, MD. 2015, 7599–7600.
[3]	International Conference on Harmonisation. Impurities in New Drug Substances Q3A(R2). 2006.
[4]	International Conference on Harmonisation. Impurities in New Drug Products Q3B(R2). 2006.
[5]	Krstulovic, A.M.; Lee, C.R.; Firmin, S.; Jacquet, G.; Tessier, D. Applications of LC-MS methodology: in the development of pharmaceuticals. LC GC Eur. 2002, 15, 31–41.

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Identification of unknown impurities in triamcinolone acetonide palmitate

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