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固相萃取/液相色谱-质谱/质谱法测定山银花中5种主要黄酮苷元的含量
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作者单位
史颖珠,侯建波,谢文,姚滨滨,盛涛,胡晓莉,张辉 1.浙江大学生物系统工程与食品科学学院浙江杭州3100582.杭州海关技术中心浙江杭州3100163.浙江省检验检疫科学技术研究院浙江杭州3100164.浙江立德产品技术有限公司浙江杭州310016 
基金项目:国家重点研发计划(2017YFF0211000)
中文摘要:该文通过含有盐酸的乙醇溶液回流水解并提取,HLB固相萃取柱净化,液相色谱-质谱/质谱法检测,建立了山银花中槲皮素、木犀草素、山萘酚、芹菜素和黄芩素5种黄酮苷元含量的测定方法。实验以芦丁、木犀草苷、紫云英苷、野漆树苷和黄芩苷5种黄酮苷为代表开展研究,山银花样品经50%的乙醇溶液(含10%浓盐酸)回流2 h水解黄酮苷,同时对黄酮苷元进行提取,HLB固相萃取柱净化,采用Mightysil RP-18色谱柱分离,液相色谱-质谱/质谱法检测(电喷雾离子源、多反应监测模式、负离子扫描),外标法定量测定水解后的5种黄酮苷元含量。方法的定量下限(S/N=10)为0005 g/kg(槲皮素),001 g/kg(木犀草素和芹菜素)和005 g/kg(山萘酚和黄芩素)。在0~10 g/kg范围内,5种黄酮苷元的线性相关系数均大于0995;在山银花样品中对待测物进行3种加标水平的回收实验(加标水平相当于水解后槲皮素和木犀草素含量为:010、020、040 g/kg,山萘酚、芹菜素和黄芩素含量为:005、010、020 g/kg),方法的平均回收率704%~104%;相对标准偏差为40%~12%。该方法实现了山银花中多种主要黄酮苷元含量的同时测定,且对研究山银花药效及与黄酮类化合物的关系具有重要意义。
中文关键词:山银花  黄酮苷元  固相萃取  液相色谱-质谱/质谱法(LC-MS/MS)
 
Simultaneous Determination of 5 Main Flavone Aglycones in Lonicerae Flos by Solid Phase Extraction Purification and Liquid Chromatography Tandem Mass Spectrometry
Abstract:In this paper,an analytical method were developed for the determination of 5 main flavone aglycones including quercetin,luteolin,kaempferol,apigenin and baicalein,in Lonicerae Flos by solid phase extraction and liquid chromatography tandem mass spectrometry(SPE/LC-MS/MS).In Lonicerae Flos samples,rutin,cynaroside,astragalin,rhoifolin and baicalin were hydrolyzed and extracted by 50% ethanol solution(contained 10% hydrochloric acid),refluxed for 120 min,and finally cleaned up with an HLB solid phase extraction column.The solution was separated on a Mightysil RP-18 column(150 mm×46 mm(id),3 μm),and determined by LC-MS/MS with negative electrospray ionization(ESI-) in multiple reaction monitoring(MRM) mode.The external standard method was used for the quantitation analysis of 5 main flavone aglycones.The limits of quantitation(LOQs,S/N=10) were 0005 g/kg for quercetin,001 g/kg for luteolin and apigenin,and 005 g/kg for kaempferol and baicalein.Single laboratory method validation data were determined,and the calibration standard curves for 5 flavone aglycones were linear in the range of 0-10 g/kg with correlation coefficients more than 0995.The recoveries,at there spiked levels of 01,02,04 g/kg for quercetin and luteolin,005,01,02 g/kg for kaempferol,apigenin and baicalein after hydrolysis,ranged from 704%to 104%with relative standard deviations of 40%-12%.This method was suitable for the simultaneous determination and confirmation of flavone aglycones in Lonicerae Flos.
Key Words:Lonicerae Flos  flavone aglycones  solid phase extraction  liquid chromatography tandem mass spectrometry(LC-MS/MS)
引用本文:史颖珠,侯建波,谢文,姚滨滨,盛涛,胡晓莉,张辉.固相萃取/液相色谱-质谱/质谱法测定山银花中5种主要黄酮苷元的含量[J].分析测试学报,2021,40(3):326-332.
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