孫云波 張創峰 畢丹 田清存 崔旭盛 沈碩



摘要:目的? 建立甘草的超高液相色譜(UPLC)指紋圖譜,為其質量標準的建立提供依據。方法? 采用反相超高液相色譜法,以Waters Acquity UPLC BEH C18(1.7 μm,2.1 mm×100 mm)為色譜柱,乙腈-0.05%磷酸為流動相,梯度洗脫,流速0.4 mL/min,檢測波長分別為237、355 nm,柱溫30 ℃,進樣量2 μL,記錄時間51 min。結果? UPLC指紋圖譜的方法學考察結果符合技術要求。共標定甘草UPLC指紋圖譜的24個指紋峰,指認其中甘草酸、芹糖基異甘草苷、甘草查爾酮A、異甘草素、甘草苷、甘草素、異甘草苷、刺甘草查爾酮和光甘草定9個指紋峰。11批甘草樣品指紋圖譜在波長237 nm處的相似度為0.940~0.988,波長355 nm處的相似度為0.831~0.982。結論? 本研究建立的甘草UPLC指紋圖譜可為甘草質量標準的建立提供依據。
關鍵詞:甘草;超高液相色譜;指紋圖譜;甘草酸;相似度分析;質量標準
中圖分類號:R284.1? ? 文獻標識碼:A? ? 文章編號:1005-5304(2020)01-0068-05
DOI:10.3969/j.issn.1005-5304.201812371
Study on UPLC Fingerprints of Glycyrrhizae Radix et Rhizoma
SUN Yunbo1,2, ZHANG Chuangfeng1, BI Dan1, TIAN Qingcun3, CUI Xusheng3, SHEN Shuo1,2
1. Beijing Yiling Pharmaceutical Co., Ltd, Beijing 102600, China;
2. Hebei Province Institute of Integrated Traditional and Western Medicine, Shijiazhuang 050035, China;
3. Shijiazhuang Yiling Pharmaceutical Co., Ltd, Shijiazhuang 050035, China
Abstract: Objective To establish UPLC fingerprints of Glycyrrhizae Radix et Rhizoma, and to provide a basis to develop the quality standard. Methods RP-UPLC fingerprints were adopted, and Waters Acquity UPLC BEH C18 (1.7 ?m, 2.1 mm × 100 mm) was set as the chromatographic column. Acetonitrile-0.05% phosphoric acid was used as the mobile phase, for gradient elution; the flow rate was 0.4 mL/min; the detection wavelengths were set at 237 nm and 355 nm; the column temperature was kept at 30 ℃; the sample volume was 2 μL; the recording time was 51 min. Results The methodological findings of UPLC fingerprints met the technical standard. 24 fingerprint peaks were marked in Glycyrrhizae Radix et Rhizoma. 9 fingerprint peaks including glycyrrhizic acid, isoliquiritin apioside, licochalcone A, isoliquiritigenin, liquiritin, liquiritigenin, isoliquiritin, echinatin and glabridin were identified. The similarities of 11 batches of Glycyrrhizae Radix et Rhizoma were among 0.940–0.988 at 237 nm and among 0.831–0.982 at 355 nm. Conclusion The established UPLC fingerprints of Glycyrrhizae Radix et Rhizoma can provide basis for the establishment of its quality standard.
Keywords: Glycyrrhizae Radix et Rhizoma; UPLC; fingerprints; glycyrrhizic acid; similarity analysis; quality standards
甘草為豆科植物甘草Glycyrrhiza uralensis Fisch.、脹果甘草Glycyrrhiza inflate Bat.或光果甘草Glycyrrhiza glabra L.的干燥根和根莖,春、秋二季采挖,除去須根,曬干。甘草氣微,味甜而特殊,具有和中緩急、潤肺祛痰、止咳平喘、補脾益氣、清熱解毒、調和諸藥之功[1],為臨床常用補益藥[2]。2015年版《中華人民共和國藥典》(一部)規定以甘草苷不得少于0.50%、甘草酸不得少于2.0%作為甘草質量控制標準[1],但甘草化學成分復雜,含有甘草酸類、黃酮類、多糖類、三萜皂苷類、木質素類及氨基酸類等多種化學成分[3-5],藥理作用豐富[6-8],其藥效為多種成分共同發揮作用的結果,僅對1種黃酮類和1種皂苷類成分進行定量分析不能從整體上反映甘草的內在質量。
中藥指紋圖譜技術作為一種從整體上控制質量的手段,能很好地反映色譜峰信息量較大的中藥質量,特征圖譜則能更好地反映色譜峰信息量相對較少的中藥質量。……