基于HS-GC-MS技术的消肿Ⅰ号挥发性成分指纹图谱研究
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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-5 MS 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 ℃, hold3 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.
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-5 MS 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 ℃, hold3 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.
引文
[1]罗兰.消肿Ⅰ号方外敷治疗轻中度癌性疼痛的临床研究[D].长沙:湖北中医药大学,2010.
[2]罗兰.消肿Ⅰ号外敷治疗癌性疼痛的临床观察[J].湖北中医杂志,2010,32(5):48.
[3]杨春娣.消肿Ⅰ号治疗癌性疼痛的效果观察[J].中国临床护理,2016,8(4):351-353.
[4]李成银,罗秀丽,王琦苑,等.见肿消巴布剂治疗癌性疼痛的临床研究[J].湖北中医药大学学报,2016,18(3):87-89.
[5]王珊,柯瑾,蒲旭峰.阿魏挥发油成分GC指纹图谱研究[J].中成药,2008,30(4):472-475.
[6]盛萍,王飒,苗莉娟,等.不同方法提取的多伞阿魏挥发油化学成分及其体外抗胃癌活性比较[J].中成药,2013,35(11):2442-2448.
[7] TIAN C, XIE L Q, GUAN L I. Germination characters of the seeds of the Ferula sinkiangensis K. M. Shen[J]. Seed, 2008, 27(5):88-90.
[8] WILKEN R, VEENA M S, WANG M B, et al. Curcumin:A review of anti-cancer properties and therapeutic activity in head and neck squamous cell carcinoma[J]. Molecular Cancer, 2011,10(1):12.
[9]李健,滕亮,戴秀勇,等.阿魏挥发油微囊的制备及初步热稳定性研究[J].中国医药工业杂志,2010,41(10):748-751.
[10] ZHANG H, LU J, ZHOU L, et al. Antioxidant and antitumor effects of Ferula sinkiangensis K. M. Shen[J]. International Journal of Clinical&Experiment, 2015, 8(11):20845.
[11] AKTHAR M S, DEGAGA B, AZAM T. Antimicrobial activity of essential oils extracted from medicinal plants against the pathogenic microorganisms:A review[J]. Issues in Biological Sciences and Pharmaceutical Research, 2014,2(1):1-7.
[12] KUNNUMAKKARA A B, BORDOLOI D, PADMAVATHI G, et al. Curcumin, the golden nutraceutical:multitargeting for multiple chronic diseases[J]. British Journal of Pharmacology, 2017, 174(11):1325-1348.
[13] LATIFI G, GHANNADI A, MINAIYAN M. Anti-inflammatory effect of volatile oil and hydroalcoholic extract of Rosa damascena Mill. on acetic acid-induced colitis in rats[J]. Research in Pharmaceutical Sciences, 2015,10(6):514.
[14] ALI B, Al-WABEL N A, SHAMS S, et al. Essential oils used in aromatherapy:A systemic review[J]. Asian Pacific Journal of Tropical Biomedicine, 2015,5(8):601-611.
[15]李莉,韩国柱.中草药挥发油类透皮吸收促进作用研究进展[J].中国新药杂志,2008,17(11):914-918,946.
[16]钟秋萍,钟兆健,陈晓东,等.SHS-GC-MS联用结合保留指数分析沉香香气成分[J].医药导报,2016,35(11):1234-1249.
[17]任燕.新疆阿魏毒性的谱效关系以及Caco-2细胞模型的吸收特性研究[D].乌鲁木齐:新疆医科大学,2014.
[18]王珊,柯瑾,蒲旭峰.阿魏挥发油中仲丁基-1-丙烯基二硫化物对照品的制备[J].中国药事,2008,22(10):889-891.
[19]张晓云,许博文,仝乐,等.蒜素抗肿瘤作用机制的研究进展[J].华北理工大学学报(医学版),2017,19(2):165-167.
[2]罗兰.消肿Ⅰ号外敷治疗癌性疼痛的临床观察[J].湖北中医杂志,2010,32(5):48.
[3]杨春娣.消肿Ⅰ号治疗癌性疼痛的效果观察[J].中国临床护理,2016,8(4):351-353.
[4]李成银,罗秀丽,王琦苑,等.见肿消巴布剂治疗癌性疼痛的临床研究[J].湖北中医药大学学报,2016,18(3):87-89.
[5]王珊,柯瑾,蒲旭峰.阿魏挥发油成分GC指纹图谱研究[J].中成药,2008,30(4):472-475.
[6]盛萍,王飒,苗莉娟,等.不同方法提取的多伞阿魏挥发油化学成分及其体外抗胃癌活性比较[J].中成药,2013,35(11):2442-2448.
[7] TIAN C, XIE L Q, GUAN L I. Germination characters of the seeds of the Ferula sinkiangensis K. M. Shen[J]. Seed, 2008, 27(5):88-90.
[8] WILKEN R, VEENA M S, WANG M B, et al. Curcumin:A review of anti-cancer properties and therapeutic activity in head and neck squamous cell carcinoma[J]. Molecular Cancer, 2011,10(1):12.
[9]李健,滕亮,戴秀勇,等.阿魏挥发油微囊的制备及初步热稳定性研究[J].中国医药工业杂志,2010,41(10):748-751.
[10] ZHANG H, LU J, ZHOU L, et al. Antioxidant and antitumor effects of Ferula sinkiangensis K. M. Shen[J]. International Journal of Clinical&Experiment, 2015, 8(11):20845.
[11] AKTHAR M S, DEGAGA B, AZAM T. Antimicrobial activity of essential oils extracted from medicinal plants against the pathogenic microorganisms:A review[J]. Issues in Biological Sciences and Pharmaceutical Research, 2014,2(1):1-7.
[12] KUNNUMAKKARA A B, BORDOLOI D, PADMAVATHI G, et al. Curcumin, the golden nutraceutical:multitargeting for multiple chronic diseases[J]. British Journal of Pharmacology, 2017, 174(11):1325-1348.
[13] LATIFI G, GHANNADI A, MINAIYAN M. Anti-inflammatory effect of volatile oil and hydroalcoholic extract of Rosa damascena Mill. on acetic acid-induced colitis in rats[J]. Research in Pharmaceutical Sciences, 2015,10(6):514.
[14] ALI B, Al-WABEL N A, SHAMS S, et al. Essential oils used in aromatherapy:A systemic review[J]. Asian Pacific Journal of Tropical Biomedicine, 2015,5(8):601-611.
[15]李莉,韩国柱.中草药挥发油类透皮吸收促进作用研究进展[J].中国新药杂志,2008,17(11):914-918,946.
[16]钟秋萍,钟兆健,陈晓东,等.SHS-GC-MS联用结合保留指数分析沉香香气成分[J].医药导报,2016,35(11):1234-1249.
[17]任燕.新疆阿魏毒性的谱效关系以及Caco-2细胞模型的吸收特性研究[D].乌鲁木齐:新疆医科大学,2014.
[18]王珊,柯瑾,蒲旭峰.阿魏挥发油中仲丁基-1-丙烯基二硫化物对照品的制备[J].中国药事,2008,22(10):889-891.
[19]张晓云,许博文,仝乐,等.蒜素抗肿瘤作用机制的研究进展[J].华北理工大学学报(医学版),2017,19(2):165-167.