Institution of Fingerprints of the TCM Wenyujin by GC-MS with Separation by SFE and Study on Their Categorization by the Systematic Clustering Analysis
摘 要
收集生长于浙江省瑞安市8个产地的温郁金样品14批次,分别经清洗、冷冻干燥及碾磨粉碎,得到通过0.425 mm筛孔药筛的粉末状样品14个。称取此样品各30 g,分别按试验选定的最佳条件[萃取温度35℃,萃取压力15 MPa,萃取时间(静态30 min,动态90 min)]进行超临界流体萃取分离,所得萃取物收集于甲醇5 mL中,并进行气相色谱-质谱法(GC-MS)分析。色谱分离采用HP-5ms石英毛细管色谱柱和在50~220℃之间程序升温模式;质谱测定采用电子轰击离子源(EI),在质荷比(m/z) 50~650内进行扫描。所得总离子流色谱图中共有50多个色谱峰,选择保留时间在40 min以内的共有峰26个作为考察对象,选择保留时间为17.12 min的莪术二酮为参考峰,计算共有峰的相对保留时间α和峰面积百分比S以及各样品与S3的S值的最大差值ΔS(Max)%,并建立了14个样品的指纹图谱。根据GC-MS分析所得结果并与NIST 14谱库比对,对共有峰作出鉴定。通过SPSS 16.0软件,采用系统聚类分析法对所分析的14批次温郁金样品的指纹图谱进行分类比较。应用指纹图谱对2个市售温郁金产品作了组分鉴定和产地认定。
Abstract
Samples of the TCM wenjujin (WYJ) from 14 different batches grown in 8 cultural areas of the Rui'an city in Zhejiang Province were collected and pretreated by washing, freeze-drying and pulverizing to pass through the medicinal sieve with bore diameter of 0.425 mm, thus to otbain 14 analytical samples in powdery form. 30 g each of the 14 samples were taken and extracted separately by SFE technique under the optimized conditions of temperature at 35℃, of pressured under 15 MPa and with times of extraction of 30 min (static) and 90 min (dynamic). The extract was collected in 5 mL of CH3OH and analyzed by GC-MS. Quartz capillary chromatographic column (HP-5ms) and programmed temperature elevation mode in the temperature interval of 50℃ to 220℃ were adopted in GC separation, and EI with scanning in the range of m/z from 50 to 650 was chosen for MS determination. As shown in the TIC chromatogram, more than 50 chromatographic peaks were obtained, among which 26 peaks in common with their retention times within 40 min were selected for further examination, using the peak of the compound numbered 16 with retention time of 17.12 min as the reference peak. Values of relative retention times α, percentages of peak areas S% and ΔS(Max) of the 26 peaks in common were calculated and their fingerprints were instituted. Based on the results obtained by GC-MS, and through comparing with the data given by the data base of NIST-14, the compounds giving the 26 common peaks were characterized. The fingerprints of the 14 samples from 8 cultural areas were studied comparatively by the systematic clustering analysis using the software of SPSS 16.0, and categorization based on the cultural areas of the Wenyujin was realized. Two Wenyujin samples obtained from the market were analyzed by the proposed method, with their components identified and their cultural areas recognized.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202004003
所属栏目 工作简报
基金项目 浙江省教育科学规划研究课题(2019SCG032);浙江省自然科学基金一般项目(LY19B050002);2019浙江省新苗计划项目(2019R454002);2020杭职院科研课题(ky202013);2019年度校级教育教学改革研究项目(JG201919)
收稿日期 2019/5/24
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备注王聪,高级实验师,硕士,主要从事天然产物功能成分提取、分离和质量分析工作,165041310@qq.com
引用该论文: WANG Cong,XIE Lei,DONG Xuerui,YANG Yuxuan,ZHENG Siyue. Institution of Fingerprints of the TCM Wenyujin by GC-MS with Separation by SFE and Study on Their Categorization by the Systematic Clustering Analysis[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2020, 56(4): 389~394
王聪,谢磊,董雪瑞,杨雨萱,郑思跃. 应用超临界流体萃取分离-气相色谱-质谱分析法建立中药温郁金的指纹图谱及其系统聚类分析[J]. 理化检验-化学分册, 2020, 56(4): 389~394
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参考文献
【1】中华人民共和国药典:一部[S].[出版地不详]:中国医药科技出版社, 2015.
【2】刘晶,王光函,庞敏,等.气相色谱法测定温郁金挥发油中5种成分含量[J].中华中医药学刊, 2017,35(9):2415-2418.
【3】张军,王亮,石典花,等.4种不同药材来源郁金饮片中挥发油成分的GC-MS分析[J].中国实验方剂学杂志, 2017,23(13):1-7.
【4】麻杰,陈娟,赵冰洁,等.抗癌药物β-榄香烯及其衍生物的研究进展[J].中草药, 2018,49(5):1184-1191.
【5】JIANG S Y, LING C H, LI W, et al. Molecular mechanisms of anti-cancer activities of β-elemene:Targeting hallmarks of cancer[J]. Anti-Cancer Agents in Medicinal Chemistry, 2016,16(11):1426-1434.
【6】孙国祥,孙万阳,闫慧,等.中药整体质量控制标准体系构建和中药一致性评价步骤[J].中南药学, 2019,17(3):321-331.
【7】马铭研,陈维.超声辅助离子液体提取反相高效液相色谱法同时测定温郁金中姜黄素和吉马酮的含量[J].中国药学杂志, 2017,52(7):592-596.
【8】张军,石典花.四种不同药材来源郁金饮片中吉马酮和姜黄素含量的高效液相色谱法测定[J].时珍国医国药, 2016,27(8):1846-1849.
【9】韩超,朱振瓯,刘滨,等.微波辅助萃取-高效液相色谱-串联质谱法测定温郁金中3个姜黄素类化合物[J].药物分析杂志, 2013,33(2):185-188.
【10】刘晶,王光函,庞敏,等.气相色谱法测定温郁金挥发油中5种成分含量[J].中华中医药学刊, 2017,35(9):2415-2418.
【11】刘玉红,刘倩伶,黄志芳,等.不同基源郁金挥发油GC指纹图谱的比较[J].中国实验方剂学杂志, 2012,18(24):166-170.
【12】谢莹,杭太俊,张正行,等.4种姜黄属药材挥发油中莪术醇含量比较[J].中草药, 2001,32(7):26-28.
【13】刘艳.姜科植物的傅里叶变换红外光谱研究[D].昆明:云南师范大学, 2016.
【14】邵清松.温郁金质量评价及指纹图谱研究[D].杭州:浙江林学院, 2007.
【15】武松.SPSS实战与统计思维[M].北京:清华大学出版社, 2019.
【16】王丽丽,王聪,潘再法,等.铁皮石斛的裂解气相色谱指纹图谱及其系统聚类分析[J].色谱, 2008,26(5):613-617.
【17】王聪,王丽丽.菊花的气相色谱指纹图谱及其系统聚类分析[J].理化检验-化学分册, 2017,53(6):679-683.
【18】钱华丽,陶文沂,王利平,等.温郁金超临界萃取物的化学成分研究[J].天然产物研究与开发, 2007,19(5):814-818.
【19】国家药品监督管理局.中药注射剂指纹图谱研究的技术要求(暂行)[J].中成药, 2000,22(10):671-675.
【2】刘晶,王光函,庞敏,等.气相色谱法测定温郁金挥发油中5种成分含量[J].中华中医药学刊, 2017,35(9):2415-2418.
【3】张军,王亮,石典花,等.4种不同药材来源郁金饮片中挥发油成分的GC-MS分析[J].中国实验方剂学杂志, 2017,23(13):1-7.
【4】麻杰,陈娟,赵冰洁,等.抗癌药物β-榄香烯及其衍生物的研究进展[J].中草药, 2018,49(5):1184-1191.
【5】JIANG S Y, LING C H, LI W, et al. Molecular mechanisms of anti-cancer activities of β-elemene:Targeting hallmarks of cancer[J]. Anti-Cancer Agents in Medicinal Chemistry, 2016,16(11):1426-1434.
【6】孙国祥,孙万阳,闫慧,等.中药整体质量控制标准体系构建和中药一致性评价步骤[J].中南药学, 2019,17(3):321-331.
【7】马铭研,陈维.超声辅助离子液体提取反相高效液相色谱法同时测定温郁金中姜黄素和吉马酮的含量[J].中国药学杂志, 2017,52(7):592-596.
【8】张军,石典花.四种不同药材来源郁金饮片中吉马酮和姜黄素含量的高效液相色谱法测定[J].时珍国医国药, 2016,27(8):1846-1849.
【9】韩超,朱振瓯,刘滨,等.微波辅助萃取-高效液相色谱-串联质谱法测定温郁金中3个姜黄素类化合物[J].药物分析杂志, 2013,33(2):185-188.
【10】刘晶,王光函,庞敏,等.气相色谱法测定温郁金挥发油中5种成分含量[J].中华中医药学刊, 2017,35(9):2415-2418.
【11】刘玉红,刘倩伶,黄志芳,等.不同基源郁金挥发油GC指纹图谱的比较[J].中国实验方剂学杂志, 2012,18(24):166-170.
【12】谢莹,杭太俊,张正行,等.4种姜黄属药材挥发油中莪术醇含量比较[J].中草药, 2001,32(7):26-28.
【13】刘艳.姜科植物的傅里叶变换红外光谱研究[D].昆明:云南师范大学, 2016.
【14】邵清松.温郁金质量评价及指纹图谱研究[D].杭州:浙江林学院, 2007.
【15】武松.SPSS实战与统计思维[M].北京:清华大学出版社, 2019.
【16】王丽丽,王聪,潘再法,等.铁皮石斛的裂解气相色谱指纹图谱及其系统聚类分析[J].色谱, 2008,26(5):613-617.
【17】王聪,王丽丽.菊花的气相色谱指纹图谱及其系统聚类分析[J].理化检验-化学分册, 2017,53(6):679-683.
【18】钱华丽,陶文沂,王利平,等.温郁金超临界萃取物的化学成分研究[J].天然产物研究与开发, 2007,19(5):814-818.
【19】国家药品监督管理局.中药注射剂指纹图谱研究的技术要求(暂行)[J].中成药, 2000,22(10):671-675.
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