目的 建立痛宁凝胶的高效液相色谱-质谱(HPLC-MS)指纹图谱,为其质量控制提供依据。方法 采用Kromasil 100-5 C₁₈色谱柱(250 mm×4.6 mm,5 μm);流动相:乙腈(A)-0.1%磷酸溶液(B),梯度洗脱;检测波长:240 nm;体积流量:1.0 mL/min;柱温:30℃;进样量:10 μL。进行质谱分析时,流动相B用0.1%甲酸溶液替代。结果 测定了10 批痛宁凝胶的指纹图谱,提取18 个色谱峰作为指纹图谱共有峰,采用MS法指认了12 个共有峰,并将共有峰归属到各药材;10 批样品相似度均大于0.9。结论 该法重复性好,简便可靠,为痛宁凝胶的质量控制和评价提供了依据。

Objective To establish HPLC-MS fingerprint of Tongning Gel, and provide reference for the quality control of Tongning Gel.Methods The determination was carried out with Kromasil 100-5 C18 column (250 mm × 4.6 mm, 5 μm). The mobile phase consisted of acetonitrile (A) - 0.1% phosphoric acid solution (B) with gradient elution. The detection wavelengths were 240 nm. The flow rate was 1.0 mL/min, and the column temperature was set at 35 ℃ with injection volume of 10 μL. 0.1% Formic acid solution was used in the MS analysis instead of the mobile phase B.Results Fingerprints of 10 batches of Tongning Gel were analyzed, and 18 common peaks were marked. Twelve Common peaks were identified by MS, and attributed to the herbs. The similarity degrees of 10 batches of the samples were above 0.9.Conclusion The method is reproducible, simple, and reliable, which can be used for the quality control and evaluation of Tongning Gel.

国家重大新药创制科技重大专项(2013ZX09402203);江苏省科技支撑计划项目(BE2013661)