温郁金三种炮制品的超高效液相色谱指纹图谱及多成分测定
[UPLC fingerprint and multi-components determination of three processed products of Rhizome of Curcuma wenyujin].
作者信息
Hao Min, Lu Tu-Lin, Mao Chun-Qin, Ji De, Li Lin, Su Lian-Lin, Gu Li-Ya, Li Ping, Qin Si-Rui
机构信息
College of Pharmacy, Nanjing University of Chinese Medicine, Nanjing 210046, China.
Wuhan University, Wuhan 430072, China.
出版信息
Zhongguo Zhong Yao Za Zhi. 2018 Jun;43(11):2288-2294. doi: 10.19540/j.cnki.cjcmm.20180322.007.
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 mL·min⁻¹; column temperature was 30 °C; 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（=0.999 9）, 10.36-259（=0.998 1）, 10.54-263.5（=0.999 3）, 30.2-755（=0.999 6）and 34.38-862（=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.
通过建立超高效液相色谱（UPLC）法同时测定三种温郁金炮制品中5种倍半萜类成分并建立UPLC指纹图谱，分析三种温郁金炮制品的质量。采用Waters ACQUITY UPLC BEH C₁₈色谱柱（2.1 mm×50 mm，1.7 μm）进行成分测定，以乙腈-水为流动相进行梯度洗脱。流速为0.3 mL·min⁻¹；柱温为30℃；检测波长设定为214 nm，进样量为1 μL。采用《中药色谱指纹图谱相似度评价系统（2012.130723）》进行相似度分析，并使用simca-p14.1软件进行疏水聚类分析（HCA）、主成分分析（PCA）和正交偏最小二乘法判别分析（OPLS-DA），以研究这三种炮制品之间成分的差异。莪术烯、莪术二酮、莪术醇、吉马酮、呋喃二烯和β-榄香烯在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）和34.38 - 862（r = 0.999 9）mg·L⁻¹范围内与色谱峰面积均呈现良好的线性关系；它们的平均回收率分别为98.75%、98.69%、98.63%、99.76%和99.57%，相对标准偏差分别为2.67%、1.47%、1.29%、2.54%和0.87%。30批样品的相似度均大于0.9，表明样品一致性良好。通过HCA、PCA和OPLS-DA模式识别可将样品清晰地分为三类，分别找出了三种炮制品之间的差异色谱峰。结果表明，温郁金炮制后药理基础发生了明显变化，可为温郁金三种炮制品的临床合理应用及质量标准的制定提供科学依据。
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