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1、第9卷第23期Vol.9No.232016年12月December2016超高效液相色譜串聯(lián)三重四極桿質(zhì)譜法同時(shí)測(cè)定銀黃顆粒中16種成分含量*邰艷妮,曾繁天,周小紅,向青,許文,黃鳴清(福建中醫(yī)藥大學(xué)藥學(xué)院,福州350122)摘要:建立超高效液相色譜串聯(lián)三重四極桿質(zhì)譜(ultra-highperformanceliquidchromatography-tandemtriplequadruplemassspectrometry,UPLC-QqQ-MS/MS)法快速定量測(cè)定銀黃顆粒中16種成分(新綠原酸、綠原酸、咖啡酸、隱綠原酸、蘆丁、野黃芩苷、木犀草苷、異綠原酸B、異綠原酸A、異
2、綠原酸C、黃芩苷、漢黃芩苷、木犀草素、黃芩素、白楊素、千層紙素A)的含量。采用UPLC-QqQ-MS/MS法,并使用負(fù)離子多反應(yīng)監(jiān)測(cè)(multiplereactionmonitoring,MRM)模式進(jìn)行含量測(cè)定。色譜條件:采用WatersCORTECSC18(2.1mm×100mm,1.6μm)色譜柱,以乙腈(A)?0.1%甲酸水(B)為流動(dòng)相進(jìn)行梯度洗脫,流速0.25mL/min,柱溫45℃.16種成分在所考察濃度范圍內(nèi)線性關(guān)系良好(R>0.9952),回收率和相對(duì)標(biāo)準(zhǔn)偏差(relativestandarddeviation,RSD)分別在98.67%~100.76%和2.
3、7%~4.5%范圍內(nèi)。本研究所采用的UPLC-QqQ-MS/MS定量分析方法簡(jiǎn)便、快速、分離效果好,可作為銀黃顆粒多成分定量評(píng)價(jià)的測(cè)定方法,為全面控制銀黃顆粒的質(zhì)量提供新的技術(shù)手段。關(guān)鍵詞:中藥學(xué);銀黃顆粒;UPLC-QqQ-MS/MS;含量測(cè)定中圖分類(lèi)號(hào):R284.1文獻(xiàn)標(biāo)識(shí)碼:A文章編號(hào):1674-2850(2016)23-2470-09Simultaneousdeterminationof16componentsinYinhuanggranulesbyUPLC-QqQ-MS/MSTAIYanni,ZENGFantian,ZHOUXiaohong,XIANGQing,XUW
4、en,HUANGMingqing(SchoolofPharmacy,FujianUniversityofTraditionalChineseMedicine,Fuzhou350122,China)Abstract:Tousearapidandaccurateultra-highperformanceliquidchromatography-tandemtriplequadruplemassspectrometry(UPLC-QqQ-MS/MS)methodforthedeterminationof16maincomponents(Neochlorogenicacid,Chlor
5、ogenicacid,Caffeicacid,Cryptochlorogenicacid,Rutin,Scutellarin,Cynaroside,IsochlorogenicacidB,IsochlorogenicacidA,IsochlorogenicacidC,Baicalin,Wogonoside,Luteolin,Baicalein,Chrysin,andOroxylinA)inYinhuanggranules.TheUPLC-QqQ-MS/MSassaywasperformedonaWatersCORTECSC18(2.1mm×100mm,1.6μm)columnw
6、ithacetonitrile-water(containing0.1%formicacid)asthemobilephasebygradientelutionataflowrateof0.25mL/min;Thecolumntemperaturewassetas45℃.MSdetectionwasperformedwithmultiplereactionmonitoring(MRM)modeusingnegativeelectrosprayionization.Satisfactorylinearitywasachievedwithintheinvestigatedlinea
7、rrangeandwithfinedeterminationcoefficient(R>0.9952),theoverallrecoverieswererangedfrom98.67%to100.76%withtherelativestandarddeviation(RSD)rangingfrom2.7%to4.5%.Itisthefirstreportofsimultaneousanalysisof16majorcomponentsinYinhuanggranulesbyusingUPLC