An automated sorbentless cryogenic needle trap device (ASCNTD) was developed for the extraction of organic volatile impurities (OVIs) from solid pharmaceuticals prior to their determination by gas chromatography (GC). In this method, a new set up was designed and used to extraction of several OVIs from ceftazidime, ceftriaxone sodium and amoxicillin. For this purpose, a proper amount of the sample was transferred into the extraction vessel. The sample headspace components were started to circulate through a needle with a flow rate of 20 mL min−1. The OVIs were trapped on the inner surface of a needle placed on top of the sample by flowing liquid nitrogen. After a predetermined time, the coiled nichrome resistance wire placed into the hollow ceramic rod was heated and the trapped analytes were desorbed and swept into the GC capillary column using the carrier gas. The effective parameters such as volume of the sample vial, headspace flow rate, extraction temperature and time, and desorption conditions have been investigated. Qualification studies reveal that pyridine (as a degradation product of ceftazidime), methylene chloride, diethylamine, triethylamine, isopropyl alcohol and n-butyl acetate are the main impurities in the studied pharmaceuticals. Detected OVIs were quantitated using external standard method. The obtained relative standard deviation values were <8%, and the limits of detection (LOD) for the detected OVIs were in the range of 1–34 ng g−1.

中文翻译：

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在线无吸附剂低温针捕集萃取结合 GC-FID 分析固体药物中某些有机挥发性杂质的应用

开发了一种自动无吸附剂低温针捕集装置 (ASCNTD)，用于在通过气相色谱 (GC) 测定固体药物之前从固体药物中提取有机挥发性杂质 (OVI)。在该方法中，设计了一种新装置并用于从头孢他啶、头孢曲松钠和阿莫西林中提取几种 OVI。为此，将适量的样品转移到萃取容器中。样品顶空组分开始通过针头循环，流速为 20 mL min-1。通过流动的液氮将 OVI 捕获在放置在样品顶部的针的内表面上。在预定的时间后，放置在空心陶瓷棒中的螺旋镍铬合金电阻丝被加热，捕获的分析物被解吸并使用载气吹扫到 GC 毛细管柱中。对样品瓶的体积、顶空流速、萃取温度和时间以及解吸条件等有效参数进行了研究。鉴定研究表明，吡啶（作为头孢他啶的降解产物）、二氯甲烷、二乙胺、三乙胺、异丙醇和乙酸正丁酯是所研究药物中的主要杂质。使用外标法对检测到的 OVI 进行定量。获得的相对标准偏差值小于 8%，检测到的 OVI 的检测限 (LOD) 在 1-34 ng g-1 的范围内。对样品瓶的体积、顶空流速、萃取温度和时间以及解吸条件等有效参数进行了研究。鉴定研究表明，吡啶（作为头孢他啶的降解产物）、二氯甲烷、二乙胺、三乙胺、异丙醇和乙酸正丁酯是所研究药物中的主要杂质。使用外标法对检测到的 OVI 进行定量。获得的相对标准偏差值小于 8%，检测到的 OVI 的检测限 (LOD) 在 1-34 ng g-1 的范围内。对样品瓶的体积、顶空流速、萃取温度和时间以及解吸条件等有效参数进行了研究。鉴定研究表明，吡啶（作为头孢他啶的降解产物）、二氯甲烷、二乙胺、三乙胺、异丙醇和乙酸正丁酯是所研究药物中的主要杂质。使用外标法对检测到的 OVI 进行定量。获得的相对标准偏差值小于 8%，检测到的 OVI 的检测限 (LOD) 在 1-34 ng g-1 的范围内。异丙醇和乙酸正丁酯是所研究药物中的主要杂质。使用外标法对检测到的 OVI 进行定量。获得的相对标准偏差值小于 8%，检测到的 OVI 的检测限 (LOD) 在 1-34 ng g-1 的范围内。异丙醇和乙酸正丁酯是所研究药物中的主要杂质。使用外标法对检测到的 OVI 进行定量。获得的相对标准偏差值小于 8%，检测到的 OVI 的检测限 (LOD) 在 1-34 ng g-1 的范围内。