Quantification of Residual Organic Solvents in Clobetasol Propionate using Headspace Capillary Gas Chromatography

IF 1.2 4区化学 Q4 BIOCHEMICAL RESEARCH METHODS

Chromatographia Pub Date : 2024-02-20 DOI:10.1007/s10337-024-04313-3

Xiaoyi Shi, Shuai Li, Zhao Li, Hangri Zeng, Yi Liu, Wen Lan, Yanming Liu, Jinfeng Zheng

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Abstract

Objective

In this study, we aimed to develop a headspace capillary gas chromatography method to quantify residual methanol, acetone, methylene chloride, diisopropyl ether, ethyl acetate, and n,n-dimethylformamide (DMF), in raw clobetasol propionate.

Methods

The headspace gas chromatography method employs a chromatographic column packed with 6% cyanopropylphenyl-94% dimethylpolysiloxane as the stationary phase. The column temperature program initiated at 40 °C, was held for 10 min, then ramped up at 10 °C per minute to 220 °C, and maintained for 1 min. Nitrogen served as the carrier gas at a flow rate of 4.84 ml/min. The injection port temperature was set at 140 °C; the flame ionization detector (FID) operated at 250 °C, and the headspace equilibrium temperature was maintained at 105 °C with a 30 min equilibration time.

Results

All six residual solvents exhibited complete separation, displaying strong linearity and achieving high recovery rates. Furthermore, the residual solvent levels in the six samples tested remained comfortably below the permissible limit.

Conclusion

Our method is accurate, reliable, rapid, and sensitive, making it well-suited for the detection of organic residual solvents in raw clobetasol propionate.

Graphical Abstract

Abstract Image

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利用顶空毛细管气相色谱法定量分析丙酸氯倍他索中的残留有机溶剂

方法采用顶空毛细管气相色谱法对氯倍他索丙酸酯原料药中残留的甲醇、丙酮、二氯甲烷、二异丙基醚、乙酸乙酯和 n,n-二甲基甲酰胺（DMF）进行定量分析。色谱柱温度程序从 40 ℃ 开始，保持 10 分钟，然后以每分钟 10 ℃ 的速度升至 220 ℃，并保持 1 分钟。氮气作为载气，流速为 4.84 ml/min。进样口温度设定为 140 °C；火焰离子化检测器 (FID) 工作温度为 250 °C，顶空平衡温度保持在 105 °C，平衡时间为 30 分钟。结论我们的方法准确、可靠、快速、灵敏，非常适合检测丙酸氯倍他索原料药中的有机残留溶剂。

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来源期刊

Chromatographia 化学-分析化学

CiteScore

3.40

自引率

5.90%

发文量

103

审稿时长

2.2 months

期刊介绍： Separation sciences, in all their various forms such as chromatography, field-flow fractionation, and electrophoresis, provide some of the most powerful techniques in analytical chemistry and are applied within a number of important application areas, including archaeology, biotechnology, clinical, environmental, food, medical, petroleum, pharmaceutical, polymer and biopolymer research. Beyond serving analytical purposes, separation techniques are also used for preparative and process-scale applications. The scope and power of separation sciences is significantly extended by combination with spectroscopic detection methods (e.g., laser-based approaches, nuclear-magnetic resonance, Raman, chemiluminescence) and particularly, mass spectrometry, to create hyphenated techniques. In addition to exciting new developments in chromatography, such as ultra high-pressure systems, multidimensional separations, and high-temperature approaches, there have also been great advances in hybrid methods combining chromatography and electro-based separations, especially on the micro- and nanoscale. Integrated biological procedures (e.g., enzymatic, immunological, receptor-based assays) can also be part of the overall analytical process.