目的 建立龙血通络胶囊指纹图谱,并进行多成分定量分析,为评价龙血通络胶囊提供依据。方法 采用Kromasil C₁₈(250 mm×4.6 mm,5 μm)色谱柱,以乙腈-0.1%甲酸水溶液梯度洗脱,体积流量1.0 mL/min,柱温35 ℃,检测波长为280、325 nm。测定10批次龙血通络胶囊,建立指纹图谱,同时采用Q-TOF/MS对指纹图谱中共有峰进行指认及对部分特征峰进行定量分析。结果 得到分离度、重复性均较好的龙血通络胶囊指纹图谱,标示出18个共有峰,相似度在0.92以上;采用LC-Q-TOF/MS方法指认了16个共有峰,其中7个共有峰经对照品比对,分别为白藜芦醇、7,4'-二羟基黄酮、龙血素A、龙血素B、紫檀茋、2,6-二甲氧基-4,4'-二羟基二氢查耳酮和2-甲氧基-4,4'-二羟基二氢查耳酮,并对这7个成分进行了定量分析,平均回收率在98.47%～101.93%(RSD均小于2.27%)。结论 同时对龙血通络胶囊指纹图谱和7个指标成分进行分析,方法快速、简便、准确,可作为全面评价该制剂质量的有效方法之一。

Objective To establish an HPLC fingerprint of Longxue Tongluo Capsule (LTC), to determine the multi-components in LTC, and to provide the basis for the evaluation of LTC. Methods The Kromasil C₁₈ (250 mm × 4.6 mm, 5 μm) column was used with a mobile phase of acetonitrile-0.1% formic acid gradient elution, the flow rate was 1.0 mL/min, the column temperature was 35 ℃, and the detection wavelength was 280 and 325 nm. Ten batches of LTC were detected to eatablish fingerprints, the common peaks were identified by Q-TOF/MS, and some of the characteristic peaks were analyzed. Results The fingerprint chromatography with good resolution and reproducibility included 18 mutual peaks, and the similarity was more than 0.92. Sixteen common peaks had been identified by LC-Q-TOF/MS, seven of which were unequivocally identified via comparing the retention time, mass spectra, and MS/MS spectra data with those of the standard compounds. Then the seven maker components were identified as resveratrol, 7,4'-dihydroxy flavone, loureirin A, loureirin B, pterostilbene, 2,6-dimethoxy-4,4'-dihydroxydihydrochalcone, and 2-methoxy-4,4'-dihydroxydihydrochalcone. The seven components were quantified, and the recoveries ranged from 98.47% to 101.93% with RSD values of less than 2.27%. Conclusion The method is rapid, simple, and accurate, and can be used for the quality control of LTC.

国家科技部“重大新药创制”——现代中药创新集群与数字制药技术平台(2013ZX09402203);江苏省科技成果转化项目——脑梗塞(恢复期)治疗药物龙血通络胶囊的国际合作研发及产业化(BA2013012)