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消核糖浆的指纹图谱及含量测定研究
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| 篇名： | 消核糖浆的指纹图谱及含量测定研究 |
| TITLE： | Study on the fingerprint and content determination of Xiaohe syrup |
| 摘要： | 目的 建立消核糖浆的高效液相色谱（HPLC）指纹图谱，并测定其中10个有效成分的含量。方法以12批消核糖浆为对象，采用超高效液相色谱-串联质谱（UPLC-MS/MS）法，以AthenaC18（250mm×4.6mm，5μm）为色谱柱，以乙腈-0.1%磷酸水溶液为流动相进行梯度洗脱，流速为1.0mL/min，检测波长为210nm。色谱图导入《中药色谱指纹图谱相似度评价系统（2012A版）》建立消核糖浆指纹图谱并进行相似度评价。采用ACQUITYUPLCBEHC18（100mm×2.1mm，1.7μm）色谱柱，以0.01%甲酸乙腈-0.01%甲酸水为流动相进行梯度洗脱，流速为0.4mL/min，结合高分辨质谱仪，以电喷雾离子源进行正负离子扫描，测定12批消核糖浆中各主要成分的含量。结果12批样品共标定33个共有峰，相似度均大于0.97；确认其中10个色谱峰，分别为王不留行黄酮苷、芍药苷、阿魏酸、柚皮苷、迷迭香酸、新橙皮苷、丹酚酸B、延胡索乙素、柴胡皂苷A、柴胡皂苷D；含量测定结果显示，上述10个成分在各自的质量浓度范围内线性关系良好（R2＞0.999），其含量分别为0.35～0.64、3.15～5.61、0.11～0.17、1.68～3.17、1.59～1.90、1.15～1.64、0.78～1.48、0.11～0.26、0.06～0.13、0.33～0.61mg/mL。结论12批消核糖浆的主要成分相似但含量有所差异；本研究建立的HPLC指纹图谱和UPLC-MS/MS含量测定方法可用于消核糖浆的全面质量评价。 |
| ABSTRACT： | OBJECTIVE To establish high performance liquid chromatography （HPLC） fingerprint of Xiaohe syrup and determine the contents of 10 effective ingredients in them. METHODS With 12 batches of Xiaohe syrup as samples， ultra-high performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS） was adopted with Athena C18 （250 mm×4.6 mm， 5 μm） as the chromatographic column， acetonitrile-0.1% phosphoric acid aqueous solution as mobile phase for gradient elution. The flow rate was 1.0 mL/min， and the detection wavelength was 210 nm. Similarity Evaluation System for Traditional Chinese Medicine Chromatographic Fingerprint （2012A version） was imported to establish the fingerprint of Xiaohe syrup and evaluate the similarity. The content determination was performed on ACQUITY UPLC BEH C18（ 100 mm×2.1 mm， 1.7 μm） chromatographic column， with 0.01% formic acid acetonitrile-0.01% formic acid water as mobile phase for gradient elution at a flow rate of 0.4 mL/min； combined with high-resolution mass spectrometer， positive and negative ions were scanned with an electric spray ion source to determine the content of each main component in 12 batches of Xiaohe syrup. RESULTS A total of 33 common peaks were calibrated in 12 batches of samples， with similarities greater than 0.97； 10 chromatographic peaks were confirmed， namely flavonoid glycosides， paeoniflorin， ferulic acid， naringin， rosmarinic acid， neohesperidin， salvianolic acid B， tetrahydropalmatine， saikosaponin A， and saikosaponin D. The results of content determination showed that the above 10 components had good linear relationships within their respective mass concentration ranges （all R 2＞0.999）， with contents ranging from 0.35 to 0.64， 3.15 to 5.61， 0.11 to 0.17， 1.68 to 3.17， 1.59 to 1.90， 1.15 to 1.64， 0.78 to 1.48， 0.11 to 0.26， 0.06 to 0.13， and 0.33 to 0.61 mg/mL， respectively. CONCLUSIONS The main components of 12 batches of Xiaohe syrup are similar， but the contents vary； HPLC fingerprint and UPLC-MS/MS content determination method established in this study can be used for comprehensive quality evaluation of Xiaohe syrup. |
| 期刊： | 2024年第35卷第12期 |
| 作者： | 李娜；汪潇潇；夏婕妤；刘宇；邓剑泠；陈万一 |
| AUTHORS： | LI Na，WANG Xiaoxiao，XIA Jieyu，LIU Yu，DENG Jianling，CHEN Wanyi |
| 关键字： | 消核糖浆；指纹图谱；质量控制；含量测定；超高效液相色谱-串联质谱 |
| KEYWORDS： | Xiaohe syrup； fingerprint； quality control； content determination； UPLC-MS/MS |
| 阅读数： | 17 次 |
| 本月下载数： | 0 次 |
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