珍宝类藏族药珍珠丸系列品种中挥发性成分的GC特征图谱

Characteristic Chromatogram of Volatile Components in Tibetan Medicine Zhenzhu Pills

目的:建立藏族药珍珠丸系列品种(二十五味珍珠丸、七十味珍珠丸)中挥发性成分的特征图谱,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 DB-1毛细管柱(0.25 mm×30 m,0.25μm),进样口温度200℃,FID检测器温度320℃;柱温初始温度为60℃,保留1 min,以4℃·min^(-1)的速率升至90℃,保留1 min,再以2℃·min^(-1)的速率升至110℃,保留10 min,再以2.5℃·min^(-1)的速率升至200℃,保留5 min,最后以5℃·min^(-1)的速率升至280℃,保留8 min;载气氮气,流速3 m L·min^(-1),进样量2μL,分流比为5∶1。结果:GC特征图谱中标定的共有峰,精密度、稳定性、重复性均达到了要求(RSD<5.0%),相似度分析中,不同厂家、不同批次的样品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,可为藏族药珍珠丸系列品种的质量评价提供借鉴。

Objective： To establish a GC chromatographic fingerprint analysis method of volatile components in Tibetan medicine Zhenzhu pills（Ershiwuwei Zhenzhu Wan and Qishiwei Zhenzhu pills）,initially determine the properties of their part components,and provide experimental basis for quality control. Method：Agilent DB-1 capillary column（0. 25 mm × 30 m,0. 25 μm） was used. The injection port temperature was200 ℃; while the FID detector temperature was 320 ℃. The temperature program was as follows： the initial column temperature was 60 ℃,maintained for 1 min; then 4 ℃·min-1up to 90 ℃,maintained for 1 min; 2 ℃·min-1up to 110 ℃,maintained for 10 min; 2. 5 ℃·min-1up to 200 ℃,maintained for 5 min; and finally 5 ℃·min-1up to 280 ℃,maintained for 8 min. The carrier gas was nitrogen and its flow rate was 3 m L·min-1,with a diversion ratio of 5 ∶ 1. Result： In all common peaks in the GC characteristic chromatogram,all of their precision,stability and repeatability met the requirements（RSD5. 0%）. Analysis of similarity showed small differences in the chemical compositions from various batches of samples,but the difference in the contents and proportion of chemical compositions were obvious. Conclusion： The established GC chromatographic fingerprint method was in good separation,and can be used as a quality control method for Tibetan medicine Zhenzhu pills.