感冒清热颗粒挥发油GC特征图谱研究

Study on GC Characteristic Chromatogram of Ganmao Qingre Granules

目的建立感冒清热颗粒中挥发油的特征图谱,对其部分成分归属进行初步判定,为其全面质量评价提供依据。方法 Agilent HP-5毛细管柱(30 m×320 mm,0.25μm);进样口温度300℃,检测器温度320℃;柱温:初始温度65℃,保持5 min,1℃.min-1升至75℃,保持2 min,再以10℃.min-1升至180℃,保持10 min,然后以5℃.min-1升至300℃,保持10 min;载气为氮气;流速:3.8 ml.min-1;进样量为2μl,不分流。结果特征图谱中共标定了6个共有峰,精密度、稳定性、重复性都达到了要求(RSD<5%),相似度分析中,不同厂家、批次各成分的种类差异不大,但成分的比例和量上差异较大。结论建立的气相特征图谱中,各共有峰分离较好,大部分批次均检出胡薄荷酮及薄荷脑,两者分离效果达到要求,可为感冒清热颗粒的质量评价提供借鉴,为进一步严格规范中成药从选材到制备工艺的全过程提供一定的参考。

Objective To provide experimental evidence for quality control of Ganmao Qingre granules by establishing their characteristic chromatogram with GC and analyzing the preliminary correspondence between the peak and a particular ingredient. Methods Agilent HP-5 capillary column（30 m × 320 mm,0.25 μm） was used. The injection port temperature was 300 ℃ ;while the detector temperature was 320 ℃. The temperature program was as follows： the initial column temperature was 65℃ maintained for 5 min, then 1℃·min-1 up to 75 ℃ maintained for 2 min,10 ℃·min-1 up to 180℃ maintained for 10 rain,finally 5 ℃ ·min-1 up to 300℃ maintained for 10 min. The carrier gas was nitrogen and its flow rate was 3.8 ml .min-1. Results A total of 6 peaks, shared by all the bai- ches of Ganmao Qingre granules, were marked in the characteristic chromatographic fingerprint. Precision, stability and repeatability met requirements. Analysis of similarity showed minor difference in the categories of ingredients from various batches, but the difference in the contents and proportion of various ingredients was obvious. Conclu- sion The separation of 6 peaks was satisfactory in the GC fingerprint. Pulegone and menthol were detected in most batches and their degree of separation met the criteria.