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基于HS-GC-MS技术的消肿Ⅰ号挥发性成分指纹图谱研究 被引量:1

Study on Volatile Fingerprinting of Xiaozhong Ointment No.1 by HS-GC-MS Technology
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摘要 目的建立消肿Ⅰ号挥发性成分指纹图谱,以期为这一内病外治对抗癌性疼痛的中药制剂的进一步研究提供科学基础。方法采用顶空静态加热萃取技术提取消肿Ⅰ号低温易挥发性成分,采用顶空-气相色谱-质谱(HS-GC-MS)联用技术进行分析,使用Agilent HP-5MS毛细管色柱(0.25μm×0.25 mm×30 m)分离;程序升温:初始温度60℃,保持5 min,以10℃/min升至120℃,保持3 min,以5℃/min升至170℃,保持5 min;分流进样,进样口温度150℃,进样量1μL,载气为高纯氦气(纯度≥99.999%),载气流量1.0 mL/min,质谱条件为EI源,轰击电压70 eV,正离子模式,离子源温度230℃。结果检验10批次样品,各批次相似度均在0.90以上,得到17个共有峰,分别进行识别与归属以及相对含量的计算。结论消肿Ⅰ号挥发性成分复杂,其中主要组成成分为仲丁基-1-丙烯基二硫化物、二烯丙基二硫醚等物质,同时含许多萜类促透皮吸收剂。 Objective To develop the volatile fingerprinting of Xiaozhong Ointment No. 1, thus providing a scientific basis for further study of the external preparation against internal cancer pain relief. Methods The low temperature volatile components of Xiaozhong Ointment No. 1 were extracted by using headspace static heating extraction technology. The headspace sampling-gas chromatography-mass spectrometry (HS-GC-MS) technology was used to analyze. Agilent HP-5MS column (0.25 μm×0.25 mm×30 m) was used and temperature programmed run was conducted:initial temperature 60℃, hold 5 min, 10℃/min rise to 120℃, hold 3 min, 5℃/min rise to 170℃, hold 5 min;split injection, inlet temperature:150℃, injection volume 1.0 μL;carrier gas was high purity helium (≥ 99.999%), carrier gas flow 1.0 mL/min;mass spectrometry conditions:EI source, bombardment voltage 70 eV, positive ion mode, ion source temperature was set at 230℃. Results After analyzing 10 batches of samples, the similarity of all batches was over 0.90. 17 substances were identified and their relative contents were analyzed. Conclusion The volatile composition of Xiaozhong Ointment No. 1 is complex, and the main components are sec-butyl-cis-trans-1-propentyl disulfide, diallyl disulfide and other substances. It also contains many terpenes for transdermal absorption.
作者 孙婉瑾 金实 段雪云 闫斌 白书仙 李成银 姜楠 SUN Wanjin;JIN Shi;DUAN Xueyun;YAN Bin;BAI Shuxian;LI Chengyin;JIANG Nan(Hubei Provincial Hospital of Traditional Chinese Medicine, Wuhan, Hubei 430061, China;Hubei Province Academy of Traditional Chinese Medicine, Wuhan, Hubei 430074, China)
出处 《湖南中医药大学学报》 CAS 2019年第4期485-488,共4页 Journal of Hunan University of Chinese Medicine
基金 中央级公益性科研院所基本科研业务费专项资金资助项目(YZ-1850) 湖北省自然科学基金项目(2011CDC031)
关键词 顶空-气相-质谱联用技术 挥发性成分 指纹图谱 消肿Ⅰ号 HS-GC-MS technology volatile components fingerprint Xiaozhong Ointment No.1
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