郝敏;陆兔林;毛春芹;季德;李林;苏联麟;顾丽亚;李平;秦思睿;
HAO Min;LU Tu-lin;MAO Chun-qin;JI De;LI Lin;SU Lian-lin;GU Li-ya;LI Ping;QIN Si-rui;College of Pharmacy,Nanjing University of Chinese Medicine;Wuhan University;

• 1:南京中医药大学药学院
• 2:武汉大学

摘要(Abstract)：

建立UPLC同时测定温郁金根茎3种炮制品中5种倍半萜类化合物含量的方法,分别构建3种炮制品的UPLC指纹图谱,用于3种温郁金根茎炮制品的质量分析;采用Waters ACQUITY UPLC BEH C18色谱柱(2.1 mm×50 mm,1.7μm),乙腈-水梯度洗脱,体积流量0.3 m L·min-1;柱温30℃;检测波长214 nm;进样量1μL进行含量测定;采用中药色谱指纹图谱相似度评价系统(2012.130723版)进行相似度评价,并使用simca-p14.1软件进行HCA,PCA与OPLS-DA分析,寻找3种饮片的差异成分。莪术二酮、莪术醇、吉马酮、呋喃二烯、β-榄香烯分别在10.8~320 mg·L~(-1)(r=0.999 9),10.36~259 mg·L~(-1)(r=0.998 1),10.54~263.5 mg·L~(-1)(r=0.999 3),30.2~755 mg·L~(-1)(r=0.999 6),34.38~862 mg·L~(-1)(r=0.999 9)时与色谱峰面积线性关系良好,平均回收率分别为98.75%,98.69%,98.63%,99.76%,99.57%,RSD分别为2.7%,1.5%,1.3%,2.5%,0.87%。30批样品相似度>0.9,表明样品一致性良好,进一步对样品进行模式识别,可以明显归为3类,并分别找出了3种饮片之间的差异色谱峰。结果表明,温郁金根茎经炮制加工后物质基础发生明显变化,为3种饮片临床合理用药及质量标准的制定提供研究依据。
To analyse the quality of three processed products of Rhizome of Curcuma wenyujin by establishing an ultra performance liquid chromatography( UPLC) method for simultaneously determining five sesquiterpene components in three processed products of rhizome of C. wenyujin and establishing UPLC fingerprints. Component determination was achieved on Waters ACQUITY UPLC BEH C18 column( 2. 1 mm × 50 mm,1. 7 μm),with acetonitrile-water as mobile phase for gradient elution. The flow rate was 0. 3 m L·min-1; column temperature was 30 ℃; the detection wavelength was set at 214 nm and injection volume was 1 μL. The similarity was analyzed with " Similarity Evaluation System for Chromatographic Fingerprint of Chinese Materia Medica( 2012. 130723) ",and hydrophobic cluster analysis( HCA),principal components analysis( PCA) and orthogonal partial least squares discriminant analysis( OPLS-DA) were conducted by using simca-p14. 1 software to investigate the differences in components among these three kinds of processed products. The curzerene,curdione,curcumol,germacrone,furanodiene and β-elemene showed good linearity relationship with chromatographic peak area within the ranges of 10. 8-320( r = 0. 999 9),10. 36-259( r = 0. 998 1),10. 54-263. 5( r = 0. 999 3),30. 2-755( r = 0. 999 6) and 34. 38-862( r = 0. 999 9) mg·L~(-1),respectively; their average recoveries were 98. 75%,98. 69%,98. 63%,99. 76% and 99. 57% respectively,with RSD of 2. 67%,1. 47%,1. 29%,2. 54% and 0. 87% respectively. The similarity of 30 batches of samples was larger than 0. 9,indicating good consistency of the samples. The samples can be clearly classified into three categories for HCA,PCA and OPLS-DA pattern recognition,the differential chromatographic peak among three processed products was found respectively. The results showed that the pharmacology basis had changed obviously after processing of Rhizome of C. wenyujin,so it can provide the scientific basis for rational clinical application and establishing quality standards of three processed products of Rhizome of curcuma wenyujin.

关键词(KeyWords)： 温郁金根茎;炮制品;UPLC;含量测定;指纹图谱;质量标准
rhizome of Curcuma wenyujin;processed products;UPLC;content determination;fingerprint;quality standard

Abstract:

Keywords:

基金项目(Foundation): 国家自然科学基金项目(81673598,81473349);; 国家中医药行业专项(2015468002-2);; 国家发改委中药饮片标准化建设项目(ZYBZH-Y-SC-40)

作者(Author): 郝敏;陆兔林;毛春芹;季德;李林;苏联麟;顾丽亚;李平;秦思睿;
HAO Min;LU Tu-lin;MAO Chun-qin;JI De;LI Lin;SU Lian-lin;GU Li-ya;LI Ping;QIN Si-rui;College of Pharmacy,Nanjing University of Chinese Medicine;Wuhan University;

Email:

DOI: 10.19540/j.cnki.cjcmm.20180322.007

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