不同等级制远志饮片的质量分析
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摘要
建立不同制远志饮片商品等级的划分和质量分析方法,并对不同等级的制远志进行分析及比较,为其等级标准的制定提供参考。收集12家饮片企业的制远志样品共34批,根据其外观直径大小,将制远志分为两个等级:一等品(直径≥3.0 mm)、二等品(直径<3.0 mm)。采用薄层色谱、含量测定和指纹图谱分析方法对不同等级的制远志样品进行分析,采用偏最小二乘法-判别分析(PLS-DA)和正交偏最小二乘法-判别分析(OPLS-DA)对不同等级制远志的指纹图谱进行统计分析。结果显示,建立的薄层色谱法可以同时鉴别制远志中的三大类主要成分:糖酯、酮和皂苷类,信息量丰富,成本低廉,操作简便安全,相比现有方法具有明显优势。指标性成分含量测定结果显示制远志一等品中的远志酮Ⅲ、3,6'-二芥子酰基蔗糖和细叶远志皂苷的含量均低于二等品;指纹图谱PLS-DA和OPLS-DA分析结果表明一等品和二等品之间有显著差异,差异的成分有sibiricose A5、sibiricose A6、远志酮Ⅲ、3,6'-二芥子酰基蔗糖和tenuifoliside A等成分。
The grading and quality analysis methods for different commercial Glycyrrhiza Polygalae Radix slices were established. The qualities of different grade samples were analyzed and compared, in order to provide useful information for the formulation of the grading standards of Glycyrrhiza Polygalae Radix slices. A total of34 batches of Glycyrrhiza Polygalae Radix slice samples collected from 12 companies were divided into two grades: first-grade(diameter ≥ 3.0 mm) and second-grade(diameter < 3.0 mm). Thin-layer chromatography(TLC),multi-component content determination and fingerprint analysis were used to analyze the qualities of different grades of Glycyrrhiza Polygalae Radix slices, and the fingerprints were statistically analyzed using partial least squares-discriminant analysis(PLS-DA) and orthogonal partial least squares-discriminant analysis(OPLS-DA).The results showed that the established TLC method can simultaneously identify three major types of components,including sugar esters, xanthones, and saponins in Glycyrrhiza Polygalae Radix slices, and has obvious advantage compared to the existing methods for its rich information, low cost, and easy or safe operation. The multi-component determination showed that the contents of three index components(polygalaxanthone Ⅲ, 3,6'-disinapoyl sucrose and tenuifolin) in the first-grade products of Glycyrrhiza Polygalae Radix slices were lower than those in the secondgrade products. The results of PLS-DA and OPLS-DA indicated significant differences were observed between the first-grade and second-grade products, with sibiricose A5, sibiricose A6, polygalaxanthone Ⅲ, 3, 6'-disinapoyl sucrose and tenuifoliside A being identifies as the major differentiate markers.
The grading and quality analysis methods for different commercial Glycyrrhiza Polygalae Radix slices were established. The qualities of different grade samples were analyzed and compared, in order to provide useful information for the formulation of the grading standards of Glycyrrhiza Polygalae Radix slices. A total of34 batches of Glycyrrhiza Polygalae Radix slice samples collected from 12 companies were divided into two grades: first-grade(diameter ≥ 3.0 mm) and second-grade(diameter < 3.0 mm). Thin-layer chromatography(TLC),multi-component content determination and fingerprint analysis were used to analyze the qualities of different grades of Glycyrrhiza Polygalae Radix slices, and the fingerprints were statistically analyzed using partial least squares-discriminant analysis(PLS-DA) and orthogonal partial least squares-discriminant analysis(OPLS-DA).The results showed that the established TLC method can simultaneously identify three major types of components,including sugar esters, xanthones, and saponins in Glycyrrhiza Polygalae Radix slices, and has obvious advantage compared to the existing methods for its rich information, low cost, and easy or safe operation. The multi-component determination showed that the contents of three index components(polygalaxanthone Ⅲ, 3,6'-disinapoyl sucrose and tenuifolin) in the first-grade products of Glycyrrhiza Polygalae Radix slices were lower than those in the secondgrade products. The results of PLS-DA and OPLS-DA indicated significant differences were observed between the first-grade and second-grade products, with sibiricose A5, sibiricose A6, polygalaxanthone Ⅲ, 3, 6'-disinapoyl sucrose and tenuifoliside A being identifies as the major differentiate markers.
引文
[1] Chinese Pharmacopoeia Commission. Pharmacopoeia of the People's Republic of China(中华人民共和国药典)[S]. Part 1.2015ed. Beijing:China Medical Science Press, 2015:156.
[2] Bai GG, Yuan F, Ye H, et al. Effects of different processing methods with honey on the chemical constituents of Polygalae Radix[J]. J Chin Med Mater(中药材),2018, 41:1845-1848.
[3] Wan DG, Chen L,Liu YP, et al. Historical research on the processing of Polygalae Radix[J]. J Chin Med Mater(中药材),2005,28:233-236.
[4] Mu ET, Zhao YH, Yan P, et al. Explore the establishment of specifications and grading standards about Chinese medicinal pieces[J]. Lishizhen Med Mater Med Res(时珍国医国药),2018,29:714-716.
[5] SFDA. Specifications and Standards for 76 Kinds of Medicinal Materials(七十六种药材商品规格标准)[S]. 1984.
[6] Jing XQ, Chen TY, Zhang FS, et al. HPLC fingerprint analysis of Polygalae Radix with different commercial grades[J]. Chin J Exp Tradit Med Form(中国实验方剂学杂志),2018, 24:1-7.
[7] Wang YY,Peng L,Hu BX. Quality research and analysis of Polygala tenuifolia with different commodity grade[J]. Chin Tradit Herb Drugs(中草药),2017, 48:3833-3840.
[8] Jiang Y, Zhang N, Cui Z, et al. Fingerprint of Polygala tenuifolia by high performance liquid chromatography[J]. Acta Pharm Sin(药学学报),2006, 41:179-183.
[9] Xue Y, Li XW, Li ZY, et al. UPLC/Q-TOF MS and NMR plant metabolomics approach in studying the effect of growth year on the quality of Polygala tenuifolia[J]. Acta Pharm Sin(药学学报),2015, 50:340-347.
[10] Dong XB, Li J, Zheng Y, et al. Preparation of tenuifolin from Radix Polygalae for reference substance[J]. Tradit Chin Drug Res Clin Pharmacol(中药新药与临床药理),2007, 18:53-54.
[2] Bai GG, Yuan F, Ye H, et al. Effects of different processing methods with honey on the chemical constituents of Polygalae Radix[J]. J Chin Med Mater(中药材),2018, 41:1845-1848.
[3] Wan DG, Chen L,Liu YP, et al. Historical research on the processing of Polygalae Radix[J]. J Chin Med Mater(中药材),2005,28:233-236.
[4] Mu ET, Zhao YH, Yan P, et al. Explore the establishment of specifications and grading standards about Chinese medicinal pieces[J]. Lishizhen Med Mater Med Res(时珍国医国药),2018,29:714-716.
[5] SFDA. Specifications and Standards for 76 Kinds of Medicinal Materials(七十六种药材商品规格标准)[S]. 1984.
[6] Jing XQ, Chen TY, Zhang FS, et al. HPLC fingerprint analysis of Polygalae Radix with different commercial grades[J]. Chin J Exp Tradit Med Form(中国实验方剂学杂志),2018, 24:1-7.
[7] Wang YY,Peng L,Hu BX. Quality research and analysis of Polygala tenuifolia with different commodity grade[J]. Chin Tradit Herb Drugs(中草药),2017, 48:3833-3840.
[8] Jiang Y, Zhang N, Cui Z, et al. Fingerprint of Polygala tenuifolia by high performance liquid chromatography[J]. Acta Pharm Sin(药学学报),2006, 41:179-183.
[9] Xue Y, Li XW, Li ZY, et al. UPLC/Q-TOF MS and NMR plant metabolomics approach in studying the effect of growth year on the quality of Polygala tenuifolia[J]. Acta Pharm Sin(药学学报),2015, 50:340-347.
[10] Dong XB, Li J, Zheng Y, et al. Preparation of tenuifolin from Radix Polygalae for reference substance[J]. Tradit Chin Drug Res Clin Pharmacol(中药新药与临床药理),2007, 18:53-54.