本文選題：安眠藥　切入點(diǎn)：失眠癥　出處：《藥物分析雜志》2017年06期 　論文類型：期刊論文

【摘要】：目的:采用LC-MS對(duì)酒石酸唑吡坦片中的雜質(zhì)進(jìn)行結(jié)構(gòu)鑒定。方法:通過(guò)酸、堿、高溫、氧化和光照對(duì)酒石酸唑吡坦片中的雜質(zhì)進(jìn)行富集,采用液相色譜-超高分辨飛行時(shí)間質(zhì)譜對(duì)未知雜質(zhì)進(jìn)行鑒定,色譜柱為C_(18)(2.1 mm×100 mm,1.9μm),流動(dòng)相為10 mmol·L~(-1)乙酸銨溶液-甲醇-乙腈(53∶23∶18),采用ESI正離子模式進(jìn)行質(zhì)譜掃描。結(jié)果:結(jié)合酒石酸唑吡坦的處方工藝初步推測(cè)了6個(gè)雜質(zhì)的化學(xué)結(jié)構(gòu)。雜質(zhì)1:4-(二甲胺基)-3-(6-甲基-2-對(duì)甲苯基咪唑并[1,2-a]吡啶-3-基)-4-氧代丁酸;雜質(zhì)4:N-甲基-2-(6-甲基-2-對(duì)甲苯基咪唑并[1,2-a]吡啶-3-基)乙酰胺;雜質(zhì)5:2-羥基-N,N-二甲基-2-(6-甲基-2-對(duì)甲苯基咪唑并[1,2-a]吡啶-3-基)乙酰胺;雜質(zhì)6:N,N-二甲基-2-(6-甲基-2-對(duì)甲苯基咪唑并[1,2-a]吡啶-3-基)-2-氧代乙酰胺;雜質(zhì)7:N,N-二甲基-2-(6-甲基-2-對(duì)甲苯基-2,3-二氫咪唑并[1,2-a]吡啶-3-基)乙酰胺;雜質(zhì)8:6-甲基-2-對(duì)甲苯基咪唑并[1,2-a]吡啶-3-甲醛。它們都具有6-甲基-2-苯基咪唑并[1,2-a]吡啶的母核。結(jié)論:超高分辨飛行時(shí)間質(zhì)譜技術(shù)能夠有效地用于藥物中雜質(zhì)的鑒定,酒石酸唑吡坦雜質(zhì)研究可為其質(zhì)量控制和工藝優(yōu)化提供參考依據(jù)。
[Abstract]:Objective: to identify the impurities in zolpidem tartrate tablets by LC-MS. Methods: the impurities in zolpidem tartrate tablets were enriched by acid, alkali, high temperature, oxidation and illumination. Unknown impurities were identified by liquid chromatography-ultrahigh resolution time-of-flight mass spectrometry. The chromatographic column was Che _ (18) ~ (18) mm 脳 10 ~ (10) mmol 路L ~ (-1) mmol 路L ~ (-1) 路L ~ (-1) acetonitrile-methanol-acetonitrile 53: 23: 18. The mass spectrometry was performed by ESI positive ion mode. Results: the chemical structures of the six impurity were preliminarily inferred by combining the prescription of zolpidem tartrate with 10 mmol 路L ~ (-1) acetonitrile solution. The impurity is 1: 4-dimethylamino-6-methyl-2-methyl-2-methyl-imidazolido [1za2-a] pyridine -3-methyl-4-oxobutyric acid; Impurity 4: N- methyl-2-methyl-2-methyl-2-methyl-2-methyl-4-methyl-imidazolidazolido [1 (2-a) pyridine-3-yl) acetamide; impurity 5: 2-hydroxy-N-dimethyl-2-methyl-2-methyl-2-methyl-2-methyl-2-methyl-2-methyl-2-methyl-2-methyl-2-methyl-2-methyl-4-methyl-imidazolyl [1 (2-a] pyridyl-3-yl) acetamide; Impurity 6: N- N- dimethyl-2-oxoacetamide; impurity 7: N- N- dimethyl-2-oxoacetamide; impurity 7: N-, N-dimethyl-2-oxoacetamide; impurity 7: N-, N-dimethyl-2-oxoacetamide; impurity 7: N-, N-dimethyl-2-oxoacetamide; impurity 7: N-, N-dimethyl-2-oxo-6-methyl-2-dihydroimidazolium and [12-a] pyridine-3-yl) acetamide; Impurity 8: 6- methyl-2- p-methylimidazo [1h2a] pyridine-3-formaldehyde. They all have the parent nucleus of 6-methyl-2-phenyimidazo [1h2a] pyridine. Conclusion: ultrahigh resolution time-of-flight mass spectrometry can be used to identify impurities in drugs. The study on the impurity of zolpidem tartrate can provide reference for its quality control and process optimization.
【作者單位】： 湖南省食品藥品檢驗(yàn)研究院;
【基金】：2015年湖南省食品藥品監(jiān)督管理局食品藥品安全科技項(xiàng)目,編號(hào)湘食藥科G201507
【分類號(hào)】：O657.63;R927.1
，

本文編號(hào)：1562281