基于挥发油GC特征图谱的黄连上清片(丸、胶囊)质量评价

Quality evaluation of Huanglian Shangqing tablets(pills and granules) based on GC characteristic chromatogram of volatile oil

目的 建立黄连上清片(丸、胶囊)的GC特征图谱,重点考察黄连上清片(丸、胶囊)中含挥发油组方药材连翘、薄荷、荆芥穗的质量状况。方法 采用Agilient HP-5毛细管柱(30 m×0.32 mm,0.25μm),程序升温,分流比:5∶1,分流流量:5 mL·min^(-1),进样量:1μL,进样口温度:250℃,采用氢火焰离子化检测器,检测器温度:260℃,柱流量:1 mL·min^(-1)。采用挥发油GC色谱特征图谱及特征峰指认结合相似度分析、主成分分析对不同生产企业的样品进行质量评价。结果 建立了56家生产企业192批样品的挥发油GC色谱特征图谱,指认连翘特征色谱峰α-蒎烯、β-蒎烯,薄荷特征色谱峰薄荷脑、薄荷酮,荆芥穗特征色谱峰胡薄荷酮,发现不同生产企业黄连上清片(丸)中挥发油成分GC色谱图差异较大,部分企业产品存在指标成分色谱峰缺失的情况。结论 建立的GC色谱特征图谱能反映产品质量状况,可用于黄连上清片(丸、胶囊)的质量评价和产品质量控制;部分生产企业生产的黄连上清片(丸、胶囊)中挥发油类有效成分不足,产品质量有待提升。

Objective To establish the GC characteristic choromatogram of Huanglian Shangqing tablets (pills and granules),and to investigate the quality of the medicinal materials (Weeping Forsythia,Mentha Hyplocalyx and Herba Schizonepetae) containing volatile oil in Huanglian Shangqing tablets (pills and granules).Methods Agilient HP-5capillary column (30 m×0.32 mm,0.25μm) was used with temperature programming,the split ratio was 5∶1,the split flow was 5 mL·min^(-1),the injection volume was 1μL,and the inlet temperature was 250°C.A hydrogen flame ionization detector was used,with the detector temperature of 260°C,and the column flow was 1 mL·min^(-1).The quality of samples from different manufacturers was evaluated by using the GC characteristic choromatogram of volatile oil and the identification of characteristic peaks,combined with similarity analysis and principal component analysis.Results The characteristic chromatograms of 192 batches of samples from 56 manufacturers were established.The peaks of Weeping Forsythia,Mentha Hyplocalyx and Herba Schizonepetae were identified as α-pinene and β-pinene,menthol and menthone,and pulegone respectively.The GC choromatogram of volatile oil components in Huanglian Shangqing tablets (pills) from different manufacturers were quite different,and some peaks of indicator components in the products from a few manufacturers have missing.ConclusionThe established GC characteristic chromatograms can reflect the product quality status and can be used for the quality evaluation and product quality control of Huanglian Shangqing tablets(pills and capsules).Huanglian Shangqing tablets (pills and capsules) from some manufacturers are insufficient in the active ingredients of volatile oil,therefore,the product quality needs to be improved.