将微波无溶剂提取(SFME)与顶空气相色谱(HS-GC)在线联用,建立了中药材的微波辅助固相顶空气相色谱法(MASP-HSGC),并用该方法快速直接分析了莪术药材中的挥发性成分。研究中对色谱条件、微波作用时间、微波作用功率等因素进行了考察,并以莪术醇为标准品考察了回收率和检出限,同时测定了莪术醇在莪术药材中的含量。对采用水蒸气蒸馏法(HD)和SFME法获得的莪术挥发油进行了气相色谱-质谱(GC-MS)分析,所得结果与所建立方法的结果进行对比。结果表明:HD-GC、SFME-GC和MASP-HSGC法所测得的化合物分别为35、33和40种;3种方法测得的莪术醇含量分别为(0.294±0.015)、(0.331±0.023)和(0.297±0.009)mg/g。该法简便快速,可用于莪术中挥发性成分的分离分析。
A novel method of microwave assisted solid phase headspace gas chromatography(MASP-HSGC) was developed through online coupling of solvent-free microwave extraction(SFME) and headspace-gas chromatography via a six-way valve.The method can quickly and directly analyze the volatile compounds from solid samples with its ability of simultaneous extraction,separation and analysis without any pretreatment.The method was applied to analyze the volatile compounds of solid Curcuma.Some experimental parameters such as the chromatographic conditions,microwave power and irradiation time were studied.Curcumol was used as the standard to evaluate the recovery,the limit of detection and the contents of compounds in a Curcuma sample.The essential oils were prepared by hydrodistillation extraction(HD) and SFME separately,and analyzed by gas chromatography-mass spectrometry(GC-MS) to compare the results with those from the developed method.It showed that the numbers of compounds obtained by the three methods of HD-GC,SFME-GC and MASP-HSGC were 35,33,40 respectively.The contents of curcumol using the three methods were(0.294±0.015),(0.331±0.023),(0.297±0.009) mg/g respectively.The method was approved to be suitable for the rapid analysis of volatile components in Curcuma.