不同干燥条件对女贞子有效成分影响的初步研究
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摘要
目的采用液质联用(liquid chromatograph mass spectrometer,LC-MS)方法,分析测定不同干燥条件下女贞子中红景天苷、木犀草苷、特女贞苷和橄榄苦苷4个成分的含量,为其干燥条件和质量控制提供理论依据。方法采用Hypersll GOLD C_(18)(100 mm×2.1 mm,3μm)色谱柱,以甲醇(A)-体积分数0.1%的甲酸水(B)为流动相,梯度洗脱,流速为0.2 mL·min~(-1),柱温为25℃。结果红景天苷、木犀草苷、特女贞苷和橄榄苦苷分别在质量浓度0.38～192.08、0.01～6.95、1.14～574.42、3.59～1 798.25 mg·L~(-1)内呈现良好的线性关系(r≥0.999 4),平均加样回收率(n=6)分别为100.4%、99.91%、99.87%和100.7%,RSD分别为0.5%、1.1%、2.2%和1.0%。不同的干燥方法和不同的干燥温度对女贞子中红景天苷、木犀草苷、特女贞苷和橄榄苦苷4个成分具有一定的影响,不同干燥条件下女贞子中成分含量变化较为明显。结论建立女贞子中红景天苷、木犀草苷、特女贞苷、橄榄苦苷成分的含量测定方法,该方法可以为女贞子干燥条件和质量评价提供理论依据。
Objective To develop a liquid chromatograph mass spectrometer method for determination of salidroside,luteolin-7-O-glucoside,spcnuezhenide,oleuropein in Ligustrum Lucidum under different drying conditions,and provide a reference for the drying condition and quality control.Methods A LC-MS method for quantitative analysis was applied with Hypersll GOLD C_(18)(100 mm×2.1 mm,3 μm) column using gradient elution with methanol(A)-0.1% Formic acid water(B) as the mobile phase(0-5 min:20%A:5-25 min:20%A-60%A) at the flow rate of 0.2 mL·min~(-1),and the column temperature was set at 25 ℃.Results Good calibration linearity was achieved for salidroside,luteolin-7-O-glucoside,spcnuezhenide,oleuropein in the ranges of 0.38-192.08,0.01-6.95,1.14-574.42 and 3.59-1 798.25 mg·L~(-1),respectively(r≥0.999 4).The average recoveries(n=6) were 100.4% with RSD of 1.5%,99.91% with RSD of 1.1%,99.87% with RSD of 2.2%,100.7% with RSD of 1.0%,respectively.Different drying methods and different drying temperatures have a certain influence on the 4 components of salidroside,luteolin-7-O-glucoside,spcnuezhenide and oleuropein in Ligustrum Lucidum.the contents of various components in Ligustrum lucidum were significantly changed under different drying conditions.Conclusion The developed method is simple,well separated and precise,and provide basis for drying condition and quality control of Ligustrum Lucidum.
Objective To develop a liquid chromatograph mass spectrometer method for determination of salidroside,luteolin-7-O-glucoside,spcnuezhenide,oleuropein in Ligustrum Lucidum under different drying conditions,and provide a reference for the drying condition and quality control.Methods A LC-MS method for quantitative analysis was applied with Hypersll GOLD C_(18)(100 mm×2.1 mm,3 μm) column using gradient elution with methanol(A)-0.1% Formic acid water(B) as the mobile phase(0-5 min:20%A:5-25 min:20%A-60%A) at the flow rate of 0.2 mL·min~(-1),and the column temperature was set at 25 ℃.Results Good calibration linearity was achieved for salidroside,luteolin-7-O-glucoside,spcnuezhenide,oleuropein in the ranges of 0.38-192.08,0.01-6.95,1.14-574.42 and 3.59-1 798.25 mg·L~(-1),respectively(r≥0.999 4).The average recoveries(n=6) were 100.4% with RSD of 1.5%,99.91% with RSD of 1.1%,99.87% with RSD of 2.2%,100.7% with RSD of 1.0%,respectively.Different drying methods and different drying temperatures have a certain influence on the 4 components of salidroside,luteolin-7-O-glucoside,spcnuezhenide and oleuropein in Ligustrum Lucidum.the contents of various components in Ligustrum lucidum were significantly changed under different drying conditions.Conclusion The developed method is simple,well separated and precise,and provide basis for drying condition and quality control of Ligustrum Lucidum.
引文
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[17] 任爽,李铮,王京辉,等.中药女贞子饮片中8个成分的含量比较研究[J].药物分析杂志,2015,35(8):1393-1402.
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[21] 安开龙,李德坤,周大铮,等.不同干燥方法对五味子药材品质的影响[J].中国中药杂志,2014,39(15):2900-2906.
[22] 刘天亮,王玲洁,宋宗辉,等.橄榄苦苷的药理作用及其研究进展[J].西南国防医药,2016,26 (6):685-687.
[2] 刘亭亭,王萌.女贞子化学成分与药理作用研究进展[J].中国实验方剂学杂志,2014,20(14):228-234.
[3] 魏祥燕,王国娟,王桦影,等.女贞子药理作用研究进展[J].上海中医药杂志,2017,51(8):106-108.
[4] 徐莹.女贞子降血糖、降血脂活性及齐墩果酸衍生化研究[D].吉林农业大学,2016.
[5] 战美,周家杰,吴琪聪,等.女贞子成分抗骨质疏松的潜在作用靶点虚拟筛选[J].世界中医药,2017,7(12):1693-1697.
[6] 吴超,朱卫丰,嵇琴,等.女贞子对正常大鼠肝脏COX活性的影响及其DNA甲基化调节机制的初步研究[J].中国中药杂志,2017,12(42):2355-2360.
[7] HYE L S,SU Y B,EUN H L,et al.Liqustri lucidi Fructus inhibits hepatic injury and functions as an antioxidant by activation of AMP-activated protein kinase in vivo and in vitro[J].Chemico-Biological Interactions,2017,262(25):57-68.
[8] LYU Y,FENG X,ZHAO P L,et al.Lucidi (FLL) ethanol extract increases bone mineral density and improves bone properties in growing female rats[J].Journal of Bone and Mineral Metabolism,2014,32 (6):616-626.
[9] 章明,周莹,吴超,等.女贞子对HepG2肝癌细胞相关基因去甲基化作用的研究[J].江西中医药,2017,5(48):61-64.
[10] 宋梦晗,张学兰,李慧芬,等.LC-TOF/MS快速鉴定女贞子4种环烯醚萜苷类化合物模拟清蒸品的化学成分[J].中国实验方剂学杂志,2016,16(22):14-17.
[11] 高亮亮,雷玉兰.女贞子多糖的提取优化工艺研究[J].安徽科技学院学报,2017,31 (5):41-45.
[12] 李晓花,马小军,张忠廉,等.不同干燥条件下云木香中木香烃内酯和去氢木香内酯含量的高效液相色谱法测定[J].时珍国医国药,2016,27(3):594-595.
[13] 麻景梅,王迎春,李琛,等.不同干燥条件连翘叶茶有效成分含量比较[J].中国中医药信息杂志,2017,24 (8):76-79.
[14] 马艳芝,王晓英,张胜珍,等.不同干燥方法对柴胡有效成分含量的影响及评价[J].中药材,2015,12(38):2511-2513.
[15] 任爽.中药酸枣仁、女贞子、五味子质量标准提高研究[D].北京中医药大学,2015.
[16] 吴修红,孙泽,杨恩龙,等.酒女贞子HPLC指纹图谱的建立及多成分含量的测定[J].药物分析杂志,2016,36(2):273-277.
[17] 任爽,李铮,王京辉,等.中药女贞子饮片中8个成分的含量比较研究[J].药物分析杂志,2015,35(8):1393-1402.
[18] 蒋叶娟,姚卫峰,张丽,等.女贞子化学成分的UPLC-ESI-Q-TOF-MS分析[J].中国中药杂志,2012,37(15):2304-2308.
[19] 黄新苹,王玲,王武朝.女贞子中黄酮类化合物的提取工艺研究[J].湖北农业科学,2016,22(55):5903-5906.
[20] 姜斐.女贞子化学成分的提取分离鉴定及活性研究[D].南京中医药大学,2010.
[21] 安开龙,李德坤,周大铮,等.不同干燥方法对五味子药材品质的影响[J].中国中药杂志,2014,39(15):2900-2906.
[22] 刘天亮,王玲洁,宋宗辉,等.橄榄苦苷的药理作用及其研究进展[J].西南国防医药,2016,26 (6):685-687.