UPLC法测定香砂养胃丸中木香烃内酯及去氢木香内酯含量
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摘要
目的:建立UPLC法测定香砂养胃丸中木香烃内酯和去氢木香内酯的含量,以控制制剂中君药木香的质量。方法:采用ACQUITY UPLC BEH C_(18)(50 mm×2. 1 mm,1. 7μm)色谱柱,以乙腈-0. 1%磷酸为流动相,流速为0. 2 ml·min~(-1),测定波长为225 nm,柱温为30℃。结果:木香烃内脂、去氢木香内脂分别在1. 62～402. 98μg·ml~(-1)(r=0. 999 9)和1. 66～828. 80μg·ml~(-1)(r=0. 999 9)范围内线性关系良好,精密度、稳定性、重复性RSD均低于2. 0%,平均加样回收率分别为96. 65%(RSD=2. 05%)、92. 93%(RSD=2. 55%)。结论:该方法准确、可靠,可用于香砂养胃丸中木香烃内酯及去氢木香内酯的含量测定。
Objective: To establish a UPLC method to determine the contents of costunolide and dehydrocostuslactone in Xiangsha Yangwei pills for the quality control of radix aucklandiae,the main herb in the formula. Methods: An ACQUITY UPLC C_(18)( 50 mm ×2. 1 mm,1. 7 μm) chromatographic column was applied with acetonitrile and 0. 1% phosphoric acid as the mobile phase. The flow rate was 0. 2 ml·min~(-1),the detection wavelength was set at 225 nm,and the column temperature was 30 ℃. Results: The linear relationships of the two components were very good within the range of 1. 62-402. 98 μg·ml~(-1)( r = 0. 999 9) for costunolide and 1. 66-828. 80 μg·ml~(-1)( r = 0. 999 9) for dehydrocostulactone. The RSDs of precision,stability and repeatability were all below 2. 0%. The recovery was 96. 65%( RSD = 2. 05%) and 92. 93%( RSD = 2. 55%),respectively. Conclusion: The method is accurate and reliable,which can be used for the determination of costunolide and dehyrocostuslactone in Xiangsha Yangwei pills.
Objective: To establish a UPLC method to determine the contents of costunolide and dehydrocostuslactone in Xiangsha Yangwei pills for the quality control of radix aucklandiae,the main herb in the formula. Methods: An ACQUITY UPLC C_(18)( 50 mm ×2. 1 mm,1. 7 μm) chromatographic column was applied with acetonitrile and 0. 1% phosphoric acid as the mobile phase. The flow rate was 0. 2 ml·min~(-1),the detection wavelength was set at 225 nm,and the column temperature was 30 ℃. Results: The linear relationships of the two components were very good within the range of 1. 62-402. 98 μg·ml~(-1)( r = 0. 999 9) for costunolide and 1. 66-828. 80 μg·ml~(-1)( r = 0. 999 9) for dehydrocostulactone. The RSDs of precision,stability and repeatability were all below 2. 0%. The recovery was 96. 65%( RSD = 2. 05%) and 92. 93%( RSD = 2. 55%),respectively. Conclusion: The method is accurate and reliable,which can be used for the determination of costunolide and dehyrocostuslactone in Xiangsha Yangwei pills.
引文
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15任孝德,屠万倩.HPLC法测定香砂养胃丸中木香烃内酯的含量[J].中医研究,2007,20(8):29-30
16 Clizia G,Giorgia R,Sandra G,et al.Rapid and efficient extraction and HPLC analysis of sesquiterpene lactones from Aucklandia lappa Root[J].Nat Prod Commun,2017,12(2):213-216
2陈琴华,李鹏,易勇.高效液相色谱法测定香砂养胃片中白术内酯Ш的含量[J].医药导报,2010,29(3):365-367
3卫洪清,刘二保,吉海滨.HPLC-荧光法测定中成药中厚朴酚与和厚朴酚含量[J].石家庄学院学报,2005,7(3):1-5
4钱鑫,徐飞.HPLC法测定香砂养胃丸中α-香附酮含量[J].辽宁中医药大学学报,2013,15(4):61-62
5王青晓,高晓洁,刘瑞新,等.香砂养胃丸(水丸)质量标准改进[J].医药导报,2016,35(3):302-305
6刘晓丽,周清.高效液相色谱法测定香砂养胃丸中橙皮苷的含量[J].中国当代医药,2013,20(4):67-68
7 Guo XH,Cheng XL,Liu WX,et al.Identification of velvet antler and its mixed varieties by UPLC-QTOF-MS combined with principal component analysis[J].J Pharm Biomed Anal,2018,165:18-23
8 Xia YG,Song Y,Liang J,et al.Quality analysis of American Ginseng cultivated in Heilongjiang using UPLC-ESI-MRM-MS with chemometric methods[J].Molecules,2018,23(9):2396
9 Jorens K,Lgors K,Lauris A,et al.Evaluation of furanocoumarins from seeds of the wild parsnip(Pastinaca sativa L.s.l.)[J].JChromatogr B,2018,1105:54-66
10莫迎,李立,韦环,等.三七止痛酊质量标准的建立[J].中国药师,2018,21(11):2049-2052
11向海燕,黄艳菲,金乾,等.UPLC测定全缘叶绿绒蒿花中3种黄酮类成分[J].中国实验方剂学杂志,2018,24(1):51-55
12张晓昕.灯盏花UPLC指纹图谱含量测定及其化学成分研究[D].北京:北京中医药大学硕士学位论文,2017
13何艳梅,林虓,王雪,等.基于UPLC测定桂枝茯苓胶囊中8种活性成分的溶出度[J].中国实验方剂学杂志,2018,24(1):14-19
14龙厚宁,王洪凤,张硕,等.银黄含化滴丸UPLC指纹图谱研究[J].中药材,2017,40(7):1628-1632
15任孝德,屠万倩.HPLC法测定香砂养胃丸中木香烃内酯的含量[J].中医研究,2007,20(8):29-30
16 Clizia G,Giorgia R,Sandra G,et al.Rapid and efficient extraction and HPLC analysis of sesquiterpene lactones from Aucklandia lappa Root[J].Nat Prod Commun,2017,12(2):213-216