本文關(guān)鍵詞： 中成藥 保健品 鎮(zhèn)靜安神類化學(xué)藥品 替代對(duì)照品法 高效液相色譜-質(zhì)譜/質(zhì)譜聯(lián)用 二級(jí)質(zhì)譜庫　出處：《藥物分析雜志》2015年01期 　論文類型：期刊論文

【摘要】：目的:建立中成藥及保健品中添加鎮(zhèn)靜安神類化學(xué)藥品的HPLC-DAD及HPLC-MS/MS分析方法,建立HPLC-DAD數(shù)據(jù)庫及二級(jí)質(zhì)譜庫,并應(yīng)用分析。方法:HPLC-DAD法采用Agilent ZORBAX Eclipse Plus C8(4.6 mm×150 mm,5μm)色譜柱,0.02 mmol·L-1磷酸二氫鉀-甲醇(95∶5)為流動(dòng)相,流速1.0 m L·min-1;HPLC-MS/MS法采用Shim-Pack VP-ODS(150 mm×2.0 mm,5μm)色譜柱,0.1%甲酸-乙腈為流動(dòng)相,梯度洗脫,流速0.3 m L·min-1,質(zhì)譜檢測器以正離子和MRM方式進(jìn)行檢測。樣品以甲醇為溶劑,超聲提取。結(jié)果:HPLC-DAD法采用有效相對(duì)保留時(shí)間和紫外光譜相似度雙指標(biāo)進(jìn)行定性準(zhǔn)確可靠,相對(duì)校正因子法回收率98%~105%。優(yōu)化HPLC-MS/MS條件,確定了定性離子及建立質(zhì)譜庫的最佳質(zhì)譜條件。結(jié)論:該法快速準(zhǔn)確,適用于中成藥及保健品中非法添加鎮(zhèn)靜安神類化學(xué)藥的質(zhì)量監(jiān)控,為替代對(duì)照品法及二級(jí)質(zhì)譜庫在此類研究中提供依據(jù)。
[Abstract]:Objective: to establish a HPLC-DAD and HPLC-MS/MS analysis method for the addition of sedative and tranquilizing chemicals in Chinese patent medicine and health care products, and to establish a HPLC-DAD database and a secondary mass spectrometry library. The mobile phase was 0.02 mmol 路L ~ (-1) potassium dihydrogen phosphate and methanol 95: 5). The flow rate was 1.0 mL 路min -1 HPLC-MS / MS. The mobile phase was Shim-Pack VP-ODS(150 mm 脳 2.0 mm ~ (5 渭 m). The mobile phase consisted of 0.1% formic acid-acetonitrile. The flow rate was 0.3 mL 路min-1, and the mass spectrometer was detected by positive ion and MRM. The sample was extracted with methanol and ultrasonic. Results the effective relative retention time and UV spectral similarity were determined by using effective relative retention time and UV spectrum similarity. The recovery rate of relative correction factor method was 98 ~ 105. The HPLC-MS/MS conditions were optimized, and the optimum mass spectrometry conditions for qualitative ion and mass spectrometry library were determined. Conclusion: this method is rapid and accurate, and is suitable for the quality control of the illegal addition of sedative and tranquilizing chemicals in Chinese patent medicine and health care products. It provides the basis for replacing the reference substance method and the secondary mass spectrometry library in this kind of research.
【作者單位】： 東營市食品藥品檢驗(yàn)中心;北京中醫(yī)藥大學(xué);
【基金】：化學(xué)新藥質(zhì)量標(biāo)準(zhǔn)研究與評(píng)價(jià)技術(shù)平臺(tái)(2011ZX09303-001)
【分類號(hào)】：R927;O657.63
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本文編號(hào)：1540207