超高效液相色谱法同时测定牙膏中5种植物源活性成分
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摘要
建立了同时测定牙膏中丹皮酚(Pae)、麝香草酚(Thy)、和厚朴酚(Hon)、厚朴酚(Mag)、甘草次酸(Gly)5种植物源活性成分的超高效液相色谱方法。牙膏样品以90%甲醇为溶剂超声提取,离心取上清液过滤后进行分析,采用Waters ACQUITY UPLCHSS C_(18)(2. 1 mm×100 mm,1. 8μm)为分离柱,乙腈-0. 1%甲酸(pH 2. 8)为流动相,梯度洗脱,流速为0. 3 mL/min,二极管阵列检测器(PDA)的检测波长为275、250nm,外标法定量。结果表明,5种植物源活性成分在2～100 mg/L质量浓度范围内呈良好的线性关系,相关系数(r)均大于0. 999;检出限为0. 2～1. 0 mg/kg,定量下限为0. 8～3. 5 mg/kg;在4个加标水平下的平均回收率为90. 5%～99. 4%,相对标准偏差(RSD)为0. 7%～5. 1%。该法分析快速、重复性好、准确性好、灵敏度高,已应用于实际牙膏样品的测定。
An ultrahigh performance liquid chromatographic( UPLC) method was developed for the determination of paeonol( Pae),thymol( Thy),honokiol( Hon),magnolol( Mag) and glycyrrhetinic acid( Gly) in toothpaste. The sample was ultrasonically extracted with 90% methanol. After centrifugation and filtration,the supernatant was separated on a Waters ACQUITY UPLC~ HSS C_(18) column(2. 1 mm × 100 mm,1. 8 μm) by gradient elution at a flow rate of 0. 3 mL/min,using acetonitrile and 0. 1% formic acid( pH 2. 8) as mobile phases. The ultraviolet detection wavelength was set at 275 nm and 250 nm,respectively. Results indicated that the five botanic active constituents had good linear relationships in the range of 2-100 mg/L with their correlation coefficients( r) more than 0. 999. The limits of detection and quantitation were in the ranges of 0. 2-1. 0 mg/kg and 0. 8-3. 5mg/kg,respectively. The average recoveries at four spiked levels ranged from 90. 5% to 99. 4% with their relative standard deviations( RSDs) of 0. 7%-5. 1%. With the characteristics of rapidness,good repeatability,accuracy and sensitivity,the method was applied in the analysis on botanic active constituents in real toothpaste samples.
An ultrahigh performance liquid chromatographic( UPLC) method was developed for the determination of paeonol( Pae),thymol( Thy),honokiol( Hon),magnolol( Mag) and glycyrrhetinic acid( Gly) in toothpaste. The sample was ultrasonically extracted with 90% methanol. After centrifugation and filtration,the supernatant was separated on a Waters ACQUITY UPLC~ HSS C_(18) column(2. 1 mm × 100 mm,1. 8 μm) by gradient elution at a flow rate of 0. 3 mL/min,using acetonitrile and 0. 1% formic acid( pH 2. 8) as mobile phases. The ultraviolet detection wavelength was set at 275 nm and 250 nm,respectively. Results indicated that the five botanic active constituents had good linear relationships in the range of 2-100 mg/L with their correlation coefficients( r) more than 0. 999. The limits of detection and quantitation were in the ranges of 0. 2-1. 0 mg/kg and 0. 8-3. 5mg/kg,respectively. The average recoveries at four spiked levels ranged from 90. 5% to 99. 4% with their relative standard deviations( RSDs) of 0. 7%-5. 1%. With the characteristics of rapidness,good repeatability,accuracy and sensitivity,the method was applied in the analysis on botanic active constituents in real toothpaste samples.
引文
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[3]Gutiérrez-Larraínzar M,Rúa J,Caro I,Castro C,Arriaga D,García-Armesto M R,Valle P.Food Control,2012,26(2):555-563.
[4]SkupieńK,Oszmiański J,Kostrzewa-Nowak D,Tarasiuk J.Cancer Lett.,2006,236(2):282-291.
[5]Jiang L L,Zhang Y L,Wang C J,Zhao D D.Mod.Diagn.Treatm.(蒋丽丽,张彦龙,王春杰,赵丹丹.现代诊断与治疗),2016,27(22):4223-4224.
[6]Xue Z Z,Yan R Y,Yu S X,Cao Y Y,Shao A J,Yang B.Chin.J.Exp.Tradit.Med.Formul.(薛珍珍,晏仁义,余盛贤,曹阳阳,邵爱娟,杨滨.中国实验方剂学杂志),2014,20(22):45-49.
[7]Ye R G.Study on the Active Constituents of Glycyrrhiza Uralensis Leaves and Quantification of Bile Acids in Hei-bing-pian and Other Traditional Animal Medicines.Inner Mongolia:Inner Mongolia University(叶日贵.甘草叶活性成分研究及黑冰片等动物药材中胆汁酸成分定量.内蒙古:内蒙古大学),2016.
[8]Liu T X,Zhou L W.J.Dezhou Univ.(刘彤曦,周连文.德州学院学报),2015,31(6):38-40.
[9]Hu X L.Study on the Toxicity of Drugs in Shanghan Lun.Beijing:Beijing University of Chinese Medicine(胡小玲.《伤寒论》药物的毒性问题研究.北京:北京中医药大学),2006.
[10]Hou M,Li G.Nei Mongol J.Tradit.Chin.Med.(侯敏,李刚.内蒙古中医药),2011,15:85-86.
[11]Xue H W,Zhou C F.J.Tradit.Chin.Med.(薛红卫,周超凡.中医杂志),2011,52(4):346-348.
[12]Li J J.Hubei J.Tradit.Chin.Med.(李江健.湖北中医杂志),2005,27(12):46-47.
[13]Luo C X.Study on the Antiviral Activity of Some Essential Oils.Lanzhou:Lanzhou Jiaotong University(罗彩霞.几种植物精油体外抗病毒活性的研究.兰州:兰州交通大学),2015.
[14]QB/T 2966-2014.Functional Toothpastes.Standards for Light Industry of the Peoples Republic of China(攻效型牙膏.中华人民共和国轻工行业标准).
[15]Shi X Q.Guangzhou Chem.Ind.(石向群.广州化工),2015,43(4):145-146,173.
[16]Zhao L,Gao X H,Sun Y T.Mod.Chin.Med.(赵磊,高秀红,孙艳涛.中国现代中药),2015,17(11):1209-1211.
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[25]Gan T.Studies on the Electrochemical Determination of Sudan Red in Foodstuffs and Honokiol,Magnolol in Traditional Chinese Medicines.Wuhan:Huazhong University of Science and Technology(甘甜.电化学测定食品中苏丹红及中药中和厚朴酚与厚朴酚的研究.武汉:华中科技大学),2008.
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