目的 采用超高效液相色谱-四极杆-飞行时间质谱联用（UPLC-Q-TOF-MS）技术鉴定消痔丸中化学成分。方法 采用Waters Acquity UPLC BEH C₁₈色谱柱（100 mm×2.1 mm，1.7 μm）；流动相为0.1%甲酸水–甲醇，梯度洗脱；体积流量0.3 mL/min；柱温25 ℃；进样量5 μL。采用Waters Xevo G2 Q-Tof高分辨质谱，配备电喷雾离子源（ESI），检测模式MSE；正负离子模式，质量数扫描范围m/z 100～1 200；离子源温度100 ℃，脱溶剂气流温度250 ℃；毛细管电压正离子模式3.0 kV，负离子模式2.5 kV，样品锥孔电压40 V，锥孔气流速50 L/h，脱气流速600 L/h；内参校准液亮氨酸脑啡肽用于相对分子质量实时校正。结果 在鉴定出的193个化学成分中，包括黄酮类、有机酸类、蒽醌类、萜类、生物碱类、2-异丁基苹果酸葡萄糖氧基苄酯类、多酚类化合物，并对化合物的药材来源进行了归属。总结了木犀草素、槐角苷、大黄酸、番泻苷B、芍药苷、白术内酯II、白术内酯I、黄芪甲苷、粉防己碱和防己诺林碱、小檗碱、白芨苷、gymnoside Ⅲ、柠檬酸、2-O-没食子酰葡萄糖的裂解方式。结论 UPLC-Q-TOF-MS技术可对消痔丸中主要成分进行鉴定，为消痔丸的质量控制、物质基础研究提供依据。

Objective To identify the chemical composition in Xiaozhi Pills using UPLC-Q-TOF-MS method. Methods The Waters Acquity UPLC BEH C₁₈ column (100 mm×2.1 mm, 1.7 μm) was used. The mobile phase was 0.1% formic acid solution - methanol, with gradient elution at a flow rate of 0.3 mL/min, the column temperature was 25 ℃, and the injection volume was 5 μL. The Waters Xevo G2 Q-Tof high resolution mass spectrometry was used, equipped with an electric spray ion source (ESI), and the detection mode was MSE. Positive and negative ion mode was adopted, with a mass scanning range of m/z 100 — 1 200. Ion source temperature was 100 ℃, desolvation gas flow temperature was 250 ℃, capillary voltage in positive ion mode was 3.0 kV, and negative ion mode was 2.5 kV. The sample cone voltage was 40 V, cone gas flow rate was 50 L/h, and degassing flow rate was 600 L/h. Internal reference leucine enkephalin solution was used for real-time correction of relative molecular weight. Results 193 Chemical components were identified, including flavonoids, organic acids, anthraquinones, terpenoids, alkaloids, 2-isobutyl malate glucoside benzyl esters, polyphenols, and their medicinal sources were attributed. The fragmentation modes of luteolin, sophoricoside, rhein, sennoside B, paeoniflorin, atractylenolide II, atractylenolide I, astragaloside IV, tetrandrine and fangchinoline, berberine, militarine, gymnoside Ⅲ, citric acid, and 2-O-galloylglucose were summarized. Conclusion UPLC-Q-TOF-MS technology can identify the main components in Xiaozhi Pills, providing a basis for quality control and material basis research of Xiaozhi Pills.

R284.1

2025年创新驱动助力工程项目（GXH20250325-12）