基于气相色谱-声表面波联用技术(GC-SAW)快速分析中药姜黄品质的方法学研究

Methodological Research on Rapid Analysis of the Quality of Rhizoma Curcumae Longae Based on GC-SAW

目的建立中药姜黄品质评价的气相色谱-声表面波联用技术(GC-SAW)检测方法。方法对色谱柱升温速率、进样口温度、阀盒温度、平衡温度以及平衡时间等主要因素进行考察。结果姜黄样品测试最佳条件为:进样口温度200℃,阀温为170℃,色谱柱初始温度55℃,5℃·s^(-1)程序升温至180℃,检测器温度50℃,姜黄样品在35℃条件下平衡10 min,顶空进样测试。在该条件下,姜黄样品在7 s内能够很好的检出,保留指数1429和1497的主峰精密度良好,RSD值在12%以内,高沸点化合物(保留指数1670)的主峰精密度相对标准偏差略高,RSD值为19.2%。建立5种姜黄正品的指纹图谱,得到7组主要成分特征峰。对其中5组特征峰进行峰归属,保留指数1029、1429、1497、1514、1670的分别为桉树醇、石竹烯、α-姜烯或α-姜黄烯、β-倍半水芹烯、姜黄酮。不同来源、不同产地和不同品种的姜黄样品都含有相同成分的特征峰,但主要挥发性成分含量有所差异,伪品不含有该7组特征峰。结论气相色谱-声表面波联用技术检测中药姜黄具有较好的响应特性,方法快速、准确,能实现中药姜黄现场快速真伪鉴别。

Objective To develop a rapid detection method of Rhizoma Curcumae Longae using gas chromatography with surface acoustic wave detector(GC-SAW).Methods The main factors such as chromatographic column heating rate,inlet temperature,valve box temperature,equilibrium temperature and equilibrium time were investigated.Results The optimum conditions for sample testing of Rhizoma Curcumae Longae were:the inlet temperature was 200℃,the valve temperature was 170℃.The initial temperature of the chromatographic column was 55℃,and the temperature was increased to 180℃by 5℃·s^(-1),and the detector temperature is 50℃,the Rhizoma Curcumae Longae was equilibrated at 35℃for 10 min,and tested by headspace sampling.Under this condition,the Rhizoma Curcumae Longae sample can be well detected within 7 s,The precision of the main peaks of retention indexes 1429 and 1497 were both good,and the RSD was within 12%.The relative standard deviation of the main peak precision of high boiling point compounds(retention index 1670)was slightly higher,and the RSD value was 19.2%.The Rhizoma Curcumae Longae fingerprint was established and 7 groups of characteristic peaks of the main components of 5 Rhizoma Curcumae Longaes were obtained.The characteristic peaks with retention indices of 1029,1429,1497,1514 and 1670 were assigned,which were eucalyptol,caryophyllene,α-gingerene orα-curcumene,β-sesquiphellandrene,and curcumin.Rhizoma Curcumae Longae samples from different sources,different producing areas and different varieties all contained the characteristic peaks of the same composition,but the content of the main volatile components was different.The fake product did not contain the 7 sets of characteristic peaks.Conclusion The surface acoustic wave gas chromatograph has good response characteristics for the detection of traditional Chinese medicine Rhizoma Curcumae Longae.The Rhizoma Curcumae Longae can be detected quickly and accurately by GC-SAW.The rapid authenticity of traditional Chinese medicine Rhizoma Curcumae Longae on site was realized.