本文選題：酮咯酸氨丁三醇 + 非甾體抗炎藥　； 參考：《藥物分析雜志》2017年08期

【摘要】：目的:對國內(nèi)各廠家生產(chǎn)的酮咯酸氨丁三醇及注射液的有關物質(zhì)現(xiàn)狀進行考察,為標準提高提供依據(jù)。方法:建立液相色譜-二極管陣列檢測器-質(zhì)譜聯(lián)用法,采用C_(18)(100 mm×4.6 mm,3μm)色譜柱,以0.05 mol·L~(-1)乙酸銨溶液(甲酸調(diào)節(jié)pH至2.5)-乙腈(60∶40)為流動相,對酮咯酸氨丁三醇及注射液中有關物質(zhì)進行分離,采用二極管陣列檢測器及ESI/Q/TOF高分辨質(zhì)譜檢測器進行檢測,對檢測到的有關物質(zhì)進行結(jié)構(gòu)解析,并將有關物質(zhì)檢測結(jié)果與現(xiàn)行標準方法檢測結(jié)果進行對比。結(jié)果:在所建立的液質(zhì)條件下,酮咯酸氨丁三醇及其有關物質(zhì)分離良好,可以檢測到酮咯酸氨丁三醇合成副產(chǎn)物及降解產(chǎn)物共22個,推斷了有關物質(zhì)1、4、6、10、13、15、21和22的結(jié)構(gòu)�，F(xiàn)有酮咯酸氨丁三醇原料藥及注射液產(chǎn)品中實際存在的有關物質(zhì)有13個。現(xiàn)行標準方法對酮咯酸氨丁三醇及注射液中的有關物質(zhì)沒有漏檢。結(jié)論:液質(zhì)聯(lián)用技術能有效地分離鑒定酮咯酸氨丁三醇及注射液中的有關物質(zhì),液質(zhì)分析結(jié)果為酮咯酸氨丁三醇及注射液的質(zhì)量控制提供了參考。
[Abstract]:Objective: to investigate the current situation of ketocloroic acid aminobutanol and related substances in injection produced by domestic manufacturers, and to provide basis for improving the standard.Methods: a liquid chromatography-diode array detector / mass spectrometry method was developed. The chromatographic column was CSTP 18mm 脳 4.6mm ~ (-3) 渭 m, and the mobile phase was 0.05 mol / L ~ (-1) ammonium acetate solution (pH adjusted by formic acid to pH (2.5) -acetonitrile (60: 40)).The related substances in ketocloroic acid aminobutanol and its injection were separated and detected by diode array detector and ESI/Q/TOF high resolution mass spectrometry.The results were compared with those of the current standard method.Results: under the established liquid quality conditions, the separation of ketoclalic acid aminobutanol and its related substances was good. 22 by-products and degradation products of ketocloroic acid aminobutanol could be detected.There are 13 related substances in raw materials and injection products of ketocloroic acid aminobutanol.The current standard method has not missed the detection of related substances in ketocloroic acid aminobutanol and its injection.Conclusion: the liquid-mass spectrometry can effectively separate and identify the related substances in ketocloroic acid aminobutanol and its injection. The result of liquid quality analysis provides a reference for the quality control of ketololac aminobutanol and its injection.
【作者單位】： 江蘇省食品藥品監(jiān)督檢驗研究院;中國藥科大學藥學院;中國食品藥品檢定研究院;
【基金】：國家“重大新藥創(chuàng)制”科技重大專項(2015ZX09303001)
【分類號】：O657.63;R927.1
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本文編號：1749686