本文關(guān)鍵詞： 鹽酸左西替利嗪 有關(guān)物質(zhì)結(jié)構(gòu)鑒定 未知雜質(zhì) 雜質(zhì)二級質(zhì)譜裂解途徑 乳糖 乙醇 LC-Triple TOF/MS -[-[(-氯苯基)(苯基)甲基]哌嗪--基]乙酸 -[-[-[(-氯--羥基苯基)(苯基)甲基]哌嗪--基]乙氧基]乙酸( R)--[-[(-氯苯基)(苯　出處：《藥物分析雜志》2017年02期 　論文類型：期刊論文

【摘要】：目的:采用LC-MS技術(shù)對鹽酸左西替利嗪片中有關(guān)物質(zhì)進(jìn)行結(jié)構(gòu)鑒定。方法:采用Welch Xtimate C18色譜柱(250 mm×4.6 mm,5μm),以甲醇-四氫呋喃-磷酸鹽溶液(磷酸二氫鈉3.1 g,用水溶解稀釋至1 000 mL,用磷酸調(diào)節(jié)pH至2.9)(44.5∶5.5∶50)為流動相等度洗脫,對鹽酸左西替利嗪片中有關(guān)物質(zhì)進(jìn)行分離;應(yīng)用Kinetex C18(100 mm×n2.1 mm,1.7μm)色譜柱,以水(含0.05%甲酸)-甲醇(含0.05%甲酸)流動相梯度洗脫,采用色譜-質(zhì)譜(MS)技術(shù)測定離子準(zhǔn)確質(zhì)量并分析離子特征,結(jié)合對照品確證有關(guān)物質(zhì)結(jié)構(gòu);結(jié)合處方分析,推測未知雜質(zhì)結(jié)構(gòu),并揭示雜質(zhì)產(chǎn)生的來源。結(jié)果:在所建立的條件下,鹽酸左西替利嗪與其有關(guān)物質(zhì)分離良好,檢測出10個有關(guān)物質(zhì),并綜合分析、鑒定了有關(guān)物質(zhì)結(jié)構(gòu),推測其中最大的未知雜質(zhì)為左西替利嗪與殘留乙醇酯化生成的2-[2-[4-[(4-氯苯基)(苯基)甲基]哌嗪-1-基]乙氧基]乙酸乙酯,另2個較大未知雜質(zhì)為是左西替利嗪的羧基與乳糖不同位置的羥基產(chǎn)生的酯化產(chǎn)物(R)-2-[2-[4-[(4-氯苯基)(苯基)甲基]哌嗪-1-基]乙氧基]乙酸乳糖酯。結(jié)論:本研究為鹽酸左西替利嗪片的處方研究及制劑工藝提供指導(dǎo)。
[Abstract]:Objective: to identify the related substances in levatirizine hydrochloride tablets by LC-MS. Methods: Welch Xtimate C18 column was used. 250 mm 脳 4.6 mm. 5 渭 m, methanol-tetrahydrofuran phosphate solution (sodium dihydrogen phosphate 3.1 g) was dissolved and diluted to 1 000 mL with water. The related substances in levocetirizine hydrochloride tablets were separated by phosphoric acid to adjust pH to 4.05: 5.5: 50) as flow equal degree elution. A Kinetex C18 ~ (18) 100 mm 脳 n ~ (2. 1) mm ~ (1.7 渭 m) column was used. The mobile phase gradient elution of water (containing 0.05% formic acid and methanol (containing 0.05% formic acid) was used to determine the accurate mass of ions and analyze the ion characteristics by chromatography-mass spectrometry. To confirm the structure of the related substance in combination with the reference substance; Combined with prescription analysis, the unknown impurity structure was inferred and the origin of impurity was revealed. Results: under the established conditions, levocetirizine hydrochloride and its related substances were separated well and 10 related substances were detected. The structure of the related substances was identified, and the largest unknown impurity was estimated to be the 2-, which was formed by the esterification of levo-cetirizine with residual ethanol. [2-. [4-. [4-chlorophenyl (phenyl) methyl] piperazine] ethoxy] ethyl acetate. The other two major unknown impurities are the esterification products of levo-cetirizine carboxyl group and lactose hydroxyl group in different positions. [2-. [4-. [Conclusion: this study provides guidance for the formulation and preparation of levcetirizine hydrochloride tablets.
【作者單位】： 湖南省藥品檢驗研究院;
【分類號】：R927;O657.63
【正文快照】： 2-[4-[(4-氯苯基)(苯基)甲基]哌嗪-1-基]乙酸;2-[2-[4-[(4-氯-3-羥基苯基)(苯基)甲基]哌嗪-1-基]乙氧基]乙酸;(R)-2-[4-[(4-氯苯基)(苯基)甲基]哌嗪-1-基]乙氧基]乙酸乳糖酯;(R)-2-[4-[(4-氯苯基)(苯基)甲基]哌嗪-1-基]乙氧基]乙酸乳糖酯;2-[4-[(4-氯苯基)(苯基)甲基]哌嗪-1-

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