以UHPLC-Q-TOF/MS建立麥門冬藥材之指紋圖譜及其在中藥製劑上的應用

Fingerprint analysis of Ophiopogonis Radix and its traditional Chinese medicine preparation by ultra high performance liquid chromatography-quadrupole time of flight/mass spectrometry

中藥材麥門冬（Ophiopogon japonicus）及山麥冬（Liriope spicata）於外觀型態極為相似，本研究蒐集市售麥門冬藥材22件，山麥冬藥材2件，外觀型態及組織切片鑑定後粉碎，經70%甲醇萃取以超高效液相層析串聯四極桿/飛行式質譜儀ultra-highperformance liquid chromatography （UHPLC）/quadrupole time-of-flight （Q-TOF/MS）建立化學成分指紋圖譜。分析條件為層析管柱Agilent Poroshell 120 EC-C18 （3.0 × 150mm, 2.7 μm）移動相為水和乙腈（均含0.1 %甲酸），以0.5 mL /min流速作梯度沖提，質譜電灑法（electrospray ionization）設定為負離子模式ESI（-）。透過一級質譜測定精確分子量與二級質譜斷裂片之資訊，比對文獻資料與標準品，成功建立麥門冬類藥材指紋。麥門冬有9個指紋，分別為甲基麥冬二氫高異黃酮A （methylophiopogonanoneA）、甲基麥冬二氫高異黃酮B （methylophiopogonanone B）、甲基麥冬高異黃酮A（methylophiopogonone A）、麥冬皂苷D （ophiopogonin D）、麥冬皂苷D’ （ophiopogoninD’）、日本麥冬皂苷C （ophiopojaponin C）、麥冬黃烷酮C （ophiopogonanone C）、麥冬黃烷酮E （ophiopogonanone E）及麥冬皂苷Ra （ophiopogon Ra）。山麥冬除了含麥冬皂苷D及麥冬皂苷D’之外，另具有山麥冬專一成分山麥冬皂苷B （liriopesides B），二種藥材以上述成分作為區別，可成功的鑑別麥門冬及山麥冬藥材及多種不同劑型之相關中藥製劑，本結果可作為日後建立麥門冬檢驗方法之參考依據。

Ophiopogonis Radix and Liriopes Radix are very similar to each other in appearance. Hence this study aimed to establish an efficient and accurate way to distinguish these two species by the the chemical fingerprint of Ophiopogonis Radix. 22 specimens of Ophiopogonis Radix and 2 specimens of Liriopes Radix were collected. All samples were smashed after the identifications of morphology and tissue sections, and then extracted with 10 mL of 70% methanol. An UHPLC-Q-TOF/MS method was developed for the chemical fingerprint analysis. The chromatography was carried on an Agilent Poroshell 120 EC-C18 (3.0 × 150 mm, 2.7 μm) with gradient elution consisting of 0.1 % formic Acid (v/v) and acetonitrile. The flow rate was set at 0.5 mL /min. Mass spectrometry was performed in the ESI negative ion mode. The fingerprint of Ophiopogonis Radix which composed 9 main peaks was established. The 9 characteristic components were methylophiopogonanone A, methylophiopogonanone B, methylophiopogonone A, ophiopogonin D, ophiopogonin D', ophiopojaponin C, ophiopogonanone C, ophiopogonanone E and ophiopogon Ra. The first 6 components were identified by matched MS spectra data with authentic reference standards. Liriopes Radix contained ophiopogonin D, ophiopogonin D'and liriopesides B as majoy components. Liriopesides B was a special compound in Liriopes Radix. The fingerprint of Ophiopogonis Radix was successfully employed for the identification of Ophiopogonis Radix and Liriopes Radix in herbal medicines and their preparations which were purchased from local markets. This report of the fingerprint analysis of Ophiopogonis Radix in this study can be utilized as reference for Ophiopogonis Radix and its preparation's identification.