摘要
目的:建立养殖麝香、天然麝香和人工麝香的气相色谱指纹图谱,分析三者差异,为有效控制和科学评价麝香药材的质量提供依据。方法:采用气相色谱法(GC),HP-1弹性石英毛细管柱(325℃,0. 25 mm×30 m,0. 25μm),进样口温度250℃,检测器温度280℃,载气N2,流速1 m L·min-1,分流比1∶1;程序升温(柱温80℃,保持2 min; 5℃·min-1升温至160℃,1℃·min-1升温至200℃,保持20 min,5℃·min-1升温至260℃,保持20 min),对30批养殖麝香,24批天然麝香和8批人工麝香进行分析,使用"中药色谱指纹图谱相似度评价系统"(2004A版)对色谱图进行相似度评价,并采用GC-MS联用技术鉴定指纹特征峰,离子源温度230℃,四极杆温度150℃,GC-MS接口温度280℃,电子轰击离子源,电子能量70 e V,扫描范围m/z 30～550。结果:建立了不同品种麝香的气相指纹图谱,相似度均符合规定,确定了养殖麝香17个共有化合物,天然麝香10个共有化合物及人工麝香8个共有化合物,并比较了养殖麝香、天然麝香和人工麝香的异同。结论:该方法精密度、重复性、稳定性好,所建立的指纹图谱可为麝香药材的整体质量评价提供依据。
Objective: To establish a gas chromatography( GC) fingerprints analysis method of farmed musk,natural musk and artificial musk for effective control and scientific evaluation of the quality of musk.Method: The sample was split in the 250 ℃ injection port,with 1 ∶ 1 split ratio,and separated on a Capillary column( 325 ℃,0. 25 mm × 30 m,0. 25 μm). Nitrogen was used as a carrier gas, the flow rate was1 m L·min-1. The detector temperature was 280 ℃. The temperature program was 80 ℃ for 2 min,increase by5 ℃·min-1 to 160 ℃,and by 1 ℃·min-1 to 200 ℃ for 20 min,then 5 ℃·min-1 to 260 ℃ for 20 min. GC of the30 batches of farmed musk,24 batches of natural musk and 8 batches of artificial musk were analyzed by adopting temperature programmer. The similarity evaluation system for chromatographic fingerprint of TCM( 2004 A) was used to evaluate the similarity of these chromatograms. The fingerprint peaks were identified by using GC-MS combination technology. The ion source temperature was set at 230 ℃. The quadrupole temperature was set at150 ℃. The GC-MS interface temperature was set at 280 ℃. Electron impact( EI) was used as the ionization source,and the electron energy was set at 70 e V. The scanning scope was m/z 30-550. Result: The GC fingerprints of different kind of musk were established,and the similarities all conformed to regulations. Totally 17 common compounds in farmed musk,10 common compounds in natural musk,and 8 common compounds in artificial musk were determined and compared. Conclusion: This method features a high precision,reproducibility,and stability. The established fingerprints could be used for the overall quality evaluation for musk.
引文
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