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[摘要]
目的 采用小粒径色谱柱建立哮喘颗粒(XCG) HPLC指纹图谱,同时快速测定其中7个有效成分(莫诺苷、苦杏仁苷、马钱苷、升麻素苷、5-O-维斯阿米醇苷、木兰脂素、五味子醇甲)的方法。方法 采用HPLC,色谱柱为Kromasil C18(150 mm×4.6 mm,3.5 μm);流动相为甲醇-乙腈-水;体积流量1.0 mL/min;梯度洗脱;检测波长:210 nm(苦杏仁苷、木兰脂素)、240 nm(莫诺苷、马钱苷、升麻素苷、5-O-维斯阿米醇苷、五味子醇甲及指纹图谱);柱温40℃;采用UPLC-Q-TOF/MS结合对照品对共有峰进行指认。结果 得到分离度和重现性良好的HPLC指纹图谱,标定了20个共有峰,10批样品相似度在0.90以上;采用UPLC-Q-TOF/MS对共有峰进行指认,11个成分经对照品比对,分别为莫诺苷、苦杏仁苷、马钱苷、升麻素苷、5-O-维斯阿米醇苷、木兰脂素、五味子醇甲、五味子醇乙、五味子酯甲、五味子甲素、五味子乙素,并对其中与功效相关的成分莫诺苷、苦杏仁苷、马钱苷、升麻素苷、5-O-甲基维斯阿米醇苷、木兰脂素、五味子醇甲进行定量分析,平均回收率在97.3%~103.8%(RSD均小于2.0%),10批次样品中7个成分量分别为莫诺苷0.51~0.69 mg/g,苦杏仁苷5.01~5.95 mg/g,马钱苷1.02~1.33 mg/g,升麻素苷0.35~0.45 mg/g,5-O-维斯阿米醇苷0.45~0.55 mg/g,木兰脂素0.38~0.48 mg/g,五味子醇甲0.89~1.08 mg/g,各成分量的RSD均小于11.0%。结论 建立的指纹图谱和7个成分定量测定的方法,快速、准确、可靠,可以用于XCG的质量评价。
[Key word]
[Abstract]
Objective To establish an HPLC fingerprint of Xiaochuan Granula (XCG), and to make a quantitative analysis of seven components by fused-core column. Methods Kromasil C18 (150 mm×4.6 mm, 3.5 μm) was used with the mobile phase of Methanol (A)-acetonitrile (B)-water (C), at a flow rate of 1.0 mL/min. The detection wavelength was set at 210 nm for amygdalin and magnolin, 240 nm for morroniside, loganin, prim-O-glucosylcimifugin, 4'-O-β-glucopyranosyl-5-O-methylvisamminol, schizandrin, and fingerprint; And the column temperature was maintained at 40℃. Common peaks had been identified by UPLC-Q-TOF/MS and standard compounds. Results The fingerprint chromatography included 20 mutual peaks, and the similarity was more than 0.90. Eleven chemical components were identified by UPLC-Q-TOF/MS and standard compounds, which were 3-morroniside, oxypaeoniflorin, 5-loganin, 6-prim-O-glucosylcimifugin, 9-4'-O-β-glucopyranosyl-5-O-methylvisamminol, 11-magnolin, 15-schisandrin, 16-schisandrol B, 18-schisantherin A, 19-deoxyschizandrin, and 20-γ-schizandrin B. Moreover, seven active components (morroniside, oxypaeoniflorin, loganin, prim-O-glucosylcimifugin, 4'-O-β-glucopyranosyl-5-O-methylvisamminol, magnolin, and schisandrin) were quantified and the average recovery rates ranged from 97.3% to 103.8% with RSDs less than 2.0%; Seven components in 10 batches samples were morroniside 0.51-0.69 mg/g, amygdalin 5.01-5.95 mg/g, loganin 1.02-1.33 mg/g, prim-O-glucosylcimifugin 0.35-0.45 mg/g, 4'-O-β-glucopyranosyl-5-O-methylvisamminol 0.45-0.55 mg/g, magnolin 0.38-0.48 mg/g, schisandrin 0.89-1.08 mg/g, respectively, and RSD of each component was less than 11.0%. Conclusion The method for establishing HPLC fingerprint and quantitative analysis of seven components is rapid, simple, and accurate, and can be used for the quality control of XCG.
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