UPLC-MS/MS法同时测定辛夷中12种木脂素
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摘要
目的建立超高效液相色谱-三重四级杆质谱法(UPLC-MS/MS)同时测定辛夷Magnolia biondii Pamp.中桉脂素、木兰脂素、epimagnolin、里立脂素B二甲醚、落叶松树脂醇-4′-O-β-D-葡萄糖苷、7R~*,8S~*-dihydrodehydrodiconiferyl alcohol-4-O-β-D-glucopyranoside、4,4′-dimethoxy-3′-hydr-oxy-7,9′:7′,9-diepoxylignan-3-O-β-D-glucopyranoside、3′,4-O-dimethylcedrusin、松脂醇、fargesol、辛夷脂素和conicaoside的含有量。方法辛夷60%甲醇提取物的分析采用Waters Acquity BEH C_(18)柱(50 mm×2.1 mm,1.7μm);流动相0.1%甲酸水-甲醇溶液,梯度洗脱;体积流量0.2 mL/min;柱温30℃。结果 12种成分在各自范围内线性关系良好(R~2>0.995 6),平均加样回收率为98.76%～102.32%, RSD 1.89%～2.58%。结论该方法准确稳定,重复性好,可用于辛夷的质量控制。
AIM To establish a UPLC-MS/MS method for the simultaneous content determination of eudesmin, magnolin, epimagnolin, lirioresinol B dimethyl ether, lariciresinol-4′-O-β-D-glucosi-de, 7R~*,8S~*-dihydrodehydrodiconiferyl alcohol-4-O-β-D-glucopyr-anoside, 4,4′-dimethoxy-3′-hy-droxy-7,9′:7′,9-diepoxylignan-3-O-β-D-glucopyranoside, 3′,4-O-dimethylcedrusin, pinoresinol, fargesol, fargesin and conicaoside in Magnolia biondii Pamp.METHODS The analysis of 60% methanol extract of M. biondii was performed on a 30 ℃ thermostatic Waters Acquity BEH C_(18)(50 mm×2.1 mm,1.7 μm), with the mobile phase comprising of 0.1% formic acid-methanol flowing at 0.2 mL/min in a gradient elution manner.RESULTS Twelve constituents showed good linear relationships within their own ranges(R~2>0.995 6), whose average recoveries were 98.76%-102.32% with the RSDs of 1.89%-2.58%.CONCLUSION This accurate,stable and reproducible method can be used for the quality control of M. biondii.
AIM To establish a UPLC-MS/MS method for the simultaneous content determination of eudesmin, magnolin, epimagnolin, lirioresinol B dimethyl ether, lariciresinol-4′-O-β-D-glucosi-de, 7R~*,8S~*-dihydrodehydrodiconiferyl alcohol-4-O-β-D-glucopyr-anoside, 4,4′-dimethoxy-3′-hy-droxy-7,9′:7′,9-diepoxylignan-3-O-β-D-glucopyranoside, 3′,4-O-dimethylcedrusin, pinoresinol, fargesol, fargesin and conicaoside in Magnolia biondii Pamp.METHODS The analysis of 60% methanol extract of M. biondii was performed on a 30 ℃ thermostatic Waters Acquity BEH C_(18)(50 mm×2.1 mm,1.7 μm), with the mobile phase comprising of 0.1% formic acid-methanol flowing at 0.2 mL/min in a gradient elution manner.RESULTS Twelve constituents showed good linear relationships within their own ranges(R~2>0.995 6), whose average recoveries were 98.76%-102.32% with the RSDs of 1.89%-2.58%.CONCLUSION This accurate,stable and reproducible method can be used for the quality control of M. biondii.
引文
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[15] 李宁,谭宁华,周俊.大叶仙茅中一个新的木脂素苷[J].云南植物研究,2003,25(6):711-715.
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[17] Yeo H,Chin Y W,Park S Y,et al.Lignans of Rosa multiflora roots[J].Arch Pharm Res,2004,27(3):287-290.
[18] Huang Y L,Chen C C,Chen Y P,et al.(-)-Fargesol,a new lignan from the flowers buds of Magnolia fargesii[J].Planta Med,1990,56(2):237-238.
[19] 李定祥,刘敏,周小江.野花椒中一个新的木脂素二聚体[J].中国中药杂志,2015,40(14):2843-2848.
[20] Fan C Q,Zhu X Z,Zhan Z J,et al.Lignans from Saussurea conica and their NO production suppressing activity[J].Planta Med,2006,72(7):590-595.
[2] 朱雄伟,杨晋凯,胡道伟.辛夷成分及其药理应用研究综述[J].海峡药学,2002,14(5):5-7.
[3] 张行,吴迎春,郭夫江,等.道地药材南召辛夷现状调研[J].中药材,2015,38(11):2285-2287.
[4] 王甜甜,曹赟,蒋运斌,等.中药辛夷研究进展[J].亚太传统医药,2017,13(18):74-78.
[5] 刁云宏,彭思毅,谢晓萍.辛夷复方制剂在鼻炎防治中的应用[J].中兽医学杂志,2017(4):83-84.
[6] 马羚,周兵冰,马逾英,等.武当玉兰与望春花嫁接辛夷的的抗炎镇痛作用试验[J].中国医药科学,2016,6(7):46-48.
[7] 冯卫生,王建超,何玉环,等.辛夷化学成分的研究[J].中国药学杂志,2015,50(24):2103-2106.
[8] 于培明,田智勇,许启泰,等.辛夷研究的新进展[J].时珍国医国药,2005,16(7):652-653.
[9] 韩果萍,周华凤.木脂素化合物的药理研究进展[J].陕西师范大学学报(自然科学版),2005,33(S1):142-144.
[10] 张永忠,李小莉,郭群.辛夷木脂素类成分抗血小板活化因子(PAF)作用的研究[J].湖北中医杂志,2001,23(10):7.
[11] 李小莉,张永忠.木兰脂素抗炎、抗过敏作用的实验研究[J].中草药,2002,33(11):1014-1015.
[12] Lee D H,Kwon S Y,Woo M H,et al.Phytochemical studies on Magnoliae Flos (I) isolation of lignans from the flower buds of Magnolia biondii[J].Nat Pro Sci,2013,19(2):161-165.
[13] Sugiyama M,Kikuchi M.Characterization of lariciresinol glucosides from Osmanthus asiaticus[J].Heterocycles,1993,36(1):117-121.
[14] Matsuda N,Sato H,Yaoita Y,et al.Isolation and absolute structures of the neolignan glycosides with the enantiometric aglycones from the leaves of Viburnum awabuki K.KOCH[J].Chem Pharm Bull,1996,44(5):1122-1123.
[15] 李宁,谭宁华,周俊.大叶仙茅中一个新的木脂素苷[J].云南植物研究,2003,25(6):711-715.
[16] Pieters L,de Bruyne T,Claeys M,et al.Isolation of a dihydrobenzofuran lignan from south American dragon’s blood (Croton spp.) as an inhibitor of cell proliferation[J].J Nat Prod,1993,56(6):899-906.
[17] Yeo H,Chin Y W,Park S Y,et al.Lignans of Rosa multiflora roots[J].Arch Pharm Res,2004,27(3):287-290.
[18] Huang Y L,Chen C C,Chen Y P,et al.(-)-Fargesol,a new lignan from the flowers buds of Magnolia fargesii[J].Planta Med,1990,56(2):237-238.
[19] 李定祥,刘敏,周小江.野花椒中一个新的木脂素二聚体[J].中国中药杂志,2015,40(14):2843-2848.
[20] Fan C Q,Zhu X Z,Zhan Z J,et al.Lignans from Saussurea conica and their NO production suppressing activity[J].Planta Med,2006,72(7):590-595.
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