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Quantification of Nitrite in Excipients and Chemicals: A Versatile and Highly Sensitive Method Using Headspace Gas Chromatography Coupled to Mass Spectrometry
Organic Process Research & Development ( IF 3.1 ) Pub Date : 2024-07-22 , DOI: 10.1021/acs.oprd.4c00115 Markus Baumann 1 , Kevin Näf 1
Organic Process Research & Development ( IF 3.1 ) Pub Date : 2024-07-22 , DOI: 10.1021/acs.oprd.4c00115 Markus Baumann 1 , Kevin Näf 1
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The trace level quantification of nitrite in excipients and chemicals is of major interest to the pharmaceutical industry due to the formation of carcinogenic nitrosamines from potentially present secondary amines and nitrite in the API and/or drug product. The aim of this work was the development of a method for the quantification of nitrite down to a level of 0.05 mg nitrite per kg material (ppm) that can be versatilely used for a wide range of excipients and chemicals. The detection of cyclohexene from the reaction of cyclamate with nitrite in water by gas chromatography coupled with mass spectrometry was selected due to its presumed great potential in terms of sensitivity, robustness, reliability, and specificity. The root cause for the presence of a significant blank peak, which was the key limiting factor, was identified and eliminated to achieve the desired sensitivity. Consequently, a method for the quantification of nitrite down to the targeted level of 0.05 ppm was developed and validated for 19 different excipients and chemicals. Specific sample preparation for challenging excipients and chemicals, such as magnesium stearate and carbonates, was developed and successfully applied. It was shown that the quantification range can be expanded up to 50 ppm covering a wide concentration range.
中文翻译：
赋形剂和化学品中亚硝酸盐的定量：使用顶空气相色谱与质谱联用的多功能且高灵敏度的方法
由于 API 和/或药品中可能存在的仲胺和亚硝酸盐会形成致癌亚硝胺，因此辅料和化学品中亚硝酸盐的痕量定量是制药行业的主要关注点。这项工作的目的是开发一种将亚硝酸盐定量至每公斤材料 0.05 毫克亚硝酸盐 (ppm) 的方法，该方法可广泛用于各种赋形剂和化学品。选择通过气相色谱-质谱联用技术检测甜蜜素与水中亚硝酸盐的反应中的环己烯，因为其在灵敏度、稳健性、可靠性和特异性方面具有巨大潜力。存在显着空白峰（这是关键限制因素）的根本原因已被识别并消除，以达到所需的灵敏度。因此，开发了一种将亚硝酸盐定量至 0.05 ppm 目标水平的方法，并针对 19 种不同的赋形剂和化学品进行了验证。开发并成功应用了针对具有挑战性的赋形剂和化学品（例如硬脂酸镁和碳酸盐）的特定样品制备方法。结果表明，定量范围可扩展至 50 ppm，覆盖较宽的浓度范围。
更新日期：2024-07-22
中文翻译：
赋形剂和化学品中亚硝酸盐的定量：使用顶空气相色谱与质谱联用的多功能且高灵敏度的方法
由于 API 和/或药品中可能存在的仲胺和亚硝酸盐会形成致癌亚硝胺，因此辅料和化学品中亚硝酸盐的痕量定量是制药行业的主要关注点。这项工作的目的是开发一种将亚硝酸盐定量至每公斤材料 0.05 毫克亚硝酸盐 (ppm) 的方法，该方法可广泛用于各种赋形剂和化学品。选择通过气相色谱-质谱联用技术检测甜蜜素与水中亚硝酸盐的反应中的环己烯，因为其在灵敏度、稳健性、可靠性和特异性方面具有巨大潜力。存在显着空白峰（这是关键限制因素）的根本原因已被识别并消除，以达到所需的灵敏度。因此，开发了一种将亚硝酸盐定量至 0.05 ppm 目标水平的方法，并针对 19 种不同的赋形剂和化学品进行了验证。开发并成功应用了针对具有挑战性的赋形剂和化学品（例如硬脂酸镁和碳酸盐）的特定样品制备方法。结果表明，定量范围可扩展至 50 ppm，覆盖较宽的浓度范围。
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