加压毛细管电色谱分离检测虎杖根中蒽醌类成分
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摘要
建立了加压毛细管电色谱法(p CEC)检测大黄酸、大黄素、芦荟大黄素、大黄酚、大黄素甲醚5种蒽醌类成分的方法,并对虎杖根中蒽醌类的成分进行分析。该方法采用EP-100-20/45-3-C_(18)毛细管色谱柱(总长度45 cm,有效长度20 cm,直径为100μm,ODS填料3μm)进行分离,流动相为20 mmol/L Na H2PO4(pH 4.7)-乙腈(15∶85),流动相的总流速为0.04 m L/min,分离电压为+5 k V,紫外检测波长为254 nm。结果表明,5种蒽醌类成分的检出限(S/N=3)为0.60~2.54μg/m L,在3.57~162.68μg/m L范围内线性关系良好,相关系数均不小于0.998 2。将所建立的方法用于虎杖中蒽醌类成分的分析,取得良好的实验结果,在低、中、高3个加标浓度下的回收率为91.1%~101.2%,相对标准偏差(RSD)为0.03%~3.6%。
A pressurized capillary electrochromatographic(p CEC) method was developed for the determination of the main anthraquinones,including rhein,emodin,aloe-emodin,chrysophanol and physcion in root of Polygonum cuspidatum. The separation was performed on a reversed-phase EP-100-20/45-3-C_(18)column(total length of 45 cm,effective length of 20 cm,diameter of 100 μm,ODS packing inside for 3 μm). The mobile phase was composed of 20 mmol/L Na H2PO4(pH 4. 7)-acetonitrile(15 ∶ 85) at a flow rate of 0. 04 m L/min. Under the optimum conditions including running voltage of + 5 k V,UV detection wavelength of 254 nm,the limits of detection(S/N = 3) were in the range of 0. 60-2. 54 μg/m L for rhein,aloe-emodin,emodin,chrysophanol and physcion,respectively,and the linear detection ranges were 3. 57-162. 68 μg/m L with correlation coefficients not less than 0. 998 2. The established method was used in the analysis of anthraquinones in polygonum cuspidatum with good results. The recoveries at three spiked levels ranged from 91. 1% to101. 2%,with relative standard deviations(RSD) of 0. 03%-3. 6%.
A pressurized capillary electrochromatographic(p CEC) method was developed for the determination of the main anthraquinones,including rhein,emodin,aloe-emodin,chrysophanol and physcion in root of Polygonum cuspidatum. The separation was performed on a reversed-phase EP-100-20/45-3-C_(18)column(total length of 45 cm,effective length of 20 cm,diameter of 100 μm,ODS packing inside for 3 μm). The mobile phase was composed of 20 mmol/L Na H2PO4(pH 4. 7)-acetonitrile(15 ∶ 85) at a flow rate of 0. 04 m L/min. Under the optimum conditions including running voltage of + 5 k V,UV detection wavelength of 254 nm,the limits of detection(S/N = 3) were in the range of 0. 60-2. 54 μg/m L for rhein,aloe-emodin,emodin,chrysophanol and physcion,respectively,and the linear detection ranges were 3. 57-162. 68 μg/m L with correlation coefficients not less than 0. 998 2. The established method was used in the analysis of anthraquinones in polygonum cuspidatum with good results. The recoveries at three spiked levels ranged from 91. 1% to101. 2%,with relative standard deviations(RSD) of 0. 03%-3. 6%.
引文
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[4]Xiao K,Xuan L J,Xu Y M,Bai D L.Chin.Pharm.J.(肖凯,宣利江,徐亚明,白东鲁.中国药学杂志),2003,38(1):12-15.
[5]Lu Y,Li H L,Lin M D,Chen D F.Chin.J.Chin.Mater.Med.(卢燕,李华丽,林牡丹,陈道峰.中国中药杂志),2012,37(13):1994-1997.
[6]Zhang Q F,Fu Y J,Chen J G,Shangguan X C.Mod.Food Sci.Technol.(张清峰,付莹娟,陈继光,上官新晨.现代食品科技),2014,3:216-219.
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[8]Ma R J B H T B K.Pressurized Capillary Electrochromatography for Residues Analysis of Pecticides and Veterinary Drug in Eggs.Shanghai:Shanghai Jiaotong University(玛尔江巴哈提别克.应用加压毛细管电色谱技术检测鸡蛋中农兽药残留的研究.上海:上海交通大学),2011.
[9]Cao F,Zhang W B,Yan C,Zhang Y K.Chin.J.Anal.Chem.(曹枫,张维冰,阎超,张玉奎.分析化学),2004,32(2):143-147.
[10]Zhao Y Y,Li L J,Huang W Y,Cheng H,Li Y Q,Hu Y,You L,Li L J.J.Instrum.Anal.(赵彦勇,李利军,黄文艺,程昊,李彦青,胡延,尤磊,李利军.分析测试学报),2015,34(10):1147-1151.
[11]Zheng S,Shi W J,Wang X X,Li J,Gu X,Yan C.Food Sci.(郑署,施文君,王晓曦,李静,谷雪,阎超.食品科学),2014,20:105-109.
[12]Guo Q L,Shi H L,Zhao L,Yang H M,Wang H.Food Res.Dev.(郭启雷,史海良,赵丽,杨红梅,王浩.食品研究与开发),2015,8:77-80.
[13]Wan Q Y,Ru X,Wang X X,Wang Y,Yan C.Chin.J.Anal.Chem.(万青云,茹鑫,王晓曦,王彦,闫超.分析化学),2015,7:1063-1068.
[14]Shan M,Li J,Ru X,Zheng S,Wang X X,Yan C.J.Anal.Sci.(山梅,李静,茹鑫,郑署,王晓曦,闫超.分析科学学报),2015,4:445-449.
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