目的 建立痛寧凝膠的高效液相色譜-質譜(HPLC-MS)指紋圖譜,為其質量控制提供依據。方法 采用Kromasil 100-5 C₁₈色譜柱(250 mm×4.6 mm,5 μm);流動相:乙腈(A)-0.1%磷酸溶液(B),梯度洗脫;檢測波長:240 nm;體積流量:1.0 mL/min;柱溫:30℃;進樣量:10 μL。進行質譜分析時,流動相B用0.1%甲酸溶液替代。結果 測定了10 批痛寧凝膠的指紋圖譜,提取18 個色譜峰作為指紋圖譜共有峰,采用MS法指認了12 個共有峰,并將共有峰歸屬到各藥材;10 批樣品相似度均大于0.9。結論 該法重復性好,簡便可靠,為痛寧凝膠的質量控制和評價提供了依據。

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.

國家重大新藥創(chuàng)制科技重大專項(2013ZX09402203);江蘇省科技支撐計劃項目(BE2013661)