18(50 mm×2.1 mm,1.7 μm)為色譜柱,以含0.1%乙酸0.02 mol/L醋酸銨溶液-乙腈為流動(dòng)相梯度洗脫,體積流量為0.3 mL/min;質(zhì)譜采用電噴霧離子源(ESI),多反應(yīng)監(jiān)測(cè)(MRM)模式進(jìn)行定性定量分析。結(jié)果 10種化學(xué)物質(zhì)的質(zhì)譜檢測(cè)線性范圍寬,線性關(guān)系良好,r ≥ 0.996 1,平均方法回收率為92.5%~101.8%,RSD為0.9%~3.1%,檢出限為0.001 5~0.018 μg,定量限為0.004 5~0.55 μg,27批樣品中有10批樣品檢出了非法添加的化學(xué)物質(zhì)。結(jié)論 本方法操作簡(jiǎn)單,靈敏度高,結(jié)果準(zhǔn)確,可作為抗風(fēng)濕類中成藥及保健品中非法添加化學(xué)物質(zhì)的測(cè)定方法。;Objective To establish a UPLC-MS/MS method for determination of 10 anti-rheumatic constituents illegally added in Chinese traditional medicine and health products preparation. Methods The column was ACQUITY UPLC BEHC18 (50 mm×2.1 mm, 1.7 μm), The mobile phase was acetonitrile -Ammonium acetate solution (containing 0.1% Acetic acid) with gradient elution at a flow rate of 0.3 mL/min. The ion source was electrospray ionization (ESI), Multiple-reaction monitoring (MRM) was performed to identify and quantify 10 anti-rheumatic constituents. Results 10 linear calibration curves were obtained with r ≥ 0.996 1. The recoveries were determinated at three concentration and ranged from 92.5% to 101.8%.The precision of the method was shown by RSD (n=5) ranged from 0.9% to 3.1%. The ranges of limit of detection were from 0.001 5 to 0.018 μg, and quantitation were from 0.004 5 to 0.55 μg. The illegally added chemicals were detected with 10 batches of 27 batches of samples. Conclusion The method were simple, sensitivity, accurate, and can be used to detect Anti-rheumatic constituents illegally added in Chinese traditional medicine and health products."/>

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首頁(yè) > 過刊瀏覽>2017年第40卷第11期 >2017,40(11):1576-1580. DOI:10.7501/j.issn.1674-6376.2017.11.009
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UPLC-MS/MS法測(cè)定抗風(fēng)濕中成藥及保健品中非法添加10種抗風(fēng)濕性化學(xué)成分

Detection of 10 anti-rheumatic constituents illegally added in Chinese traditional medicine and health products by UPLC-MS/MS

發(fā)布日期:2017-11-15
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