白术生、制品的DCBI-MS鉴别
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摘要
目的建立白术生、制品的解吸附电晕束离子化质谱(DCBI-MS)(秒级)快速鉴别方法。方法采用原位跟踪技术跟踪苍术酮的转化,初步探讨白术的最佳炮制温度;采用DCBI-MS法对白术生、制品的化学成分进行分析。结果白术最佳的炮制温度为120～140℃。60批样品中包括对照药材1批,生药材27批,土炒白术19批,麸炒白术13批;与生品相比较,加热炮制品中苍术酮的含量均有不同程度的降低,白术内酯Ⅱ(atractylenolideⅡ)和白术内酯Ⅲ(atractylenolideⅢ)的相对响应丰度值有显著增高;生白术的相似度为0.90～0.95,土炒白术的相似度为0.83～0.90,而麸炒白术的相似度为0.71～0.82,且可直观地将白术生品、土炒白术和麸炒白术分为三类。结论DCBI-MS法可有效跟踪炮制过程中苍术酮向白术内酯(atractylenolide)Ⅰ～Ⅲ转化的情况,获得其最佳炮制参数,并可有效辨别白术生、制品,可作为炮制条件优化的快速检测工具,为中药材的质量控制提供参考。
Objective To establish a rapid identification method for desorption corona beam ionization-mass spectrometry(DCBI-MS)(second order) of processed and unprocessed atractylodes. Methods The in situ tracking technique was used to track the transformation of atractyl ketone, and the best processing temperature of atractylodes were discussed.The chemical constituents of processed and unprocessed atractylodes were analyzed by DCBI-MS. Results The best processing temperature of atractylodes were 120-140℃. Sixty batches of samples included 1 batch of reference medicinal materials, 27 batches of raw medicinal herbs, 19 batches of earth-boiled atractylodes, and 13 batches of bran-enriched atractylodes; compared with raw products, the contents of atractyl ketone in processed products decreased to varying degrees, and the relative abundance of atractylenolide Ⅱ and atractylenolide Ⅲ increased significantly; the similarity of raw atractylodes was 0.90-0.95, the similarity of atractylodes processed with soil was 0.83-0.90, and the similarity of atractylodes processed with wheat bran was 0.71-0.82, and it can be used to visually distinguish between raw atractylodes, atractylodes processed with soil, and atractylodes processed with wheat bran. Conclusion The DCBIMS method can effectively track the transformation of atractylenolide Ⅰ, Ⅱ and Ⅲ during processing, and obtain the best processing parameters, and can effectively distinguish the processed and unprocessed atractylodes, which can be optimized as processing conditions. The rapid detection tool provides a reference for the quality control of Chinese herbal medicines.
Objective To establish a rapid identification method for desorption corona beam ionization-mass spectrometry(DCBI-MS)(second order) of processed and unprocessed atractylodes. Methods The in situ tracking technique was used to track the transformation of atractyl ketone, and the best processing temperature of atractylodes were discussed.The chemical constituents of processed and unprocessed atractylodes were analyzed by DCBI-MS. Results The best processing temperature of atractylodes were 120-140℃. Sixty batches of samples included 1 batch of reference medicinal materials, 27 batches of raw medicinal herbs, 19 batches of earth-boiled atractylodes, and 13 batches of bran-enriched atractylodes; compared with raw products, the contents of atractyl ketone in processed products decreased to varying degrees, and the relative abundance of atractylenolide Ⅱ and atractylenolide Ⅲ increased significantly; the similarity of raw atractylodes was 0.90-0.95, the similarity of atractylodes processed with soil was 0.83-0.90, and the similarity of atractylodes processed with wheat bran was 0.71-0.82, and it can be used to visually distinguish between raw atractylodes, atractylodes processed with soil, and atractylodes processed with wheat bran. Conclusion The DCBIMS method can effectively track the transformation of atractylenolide Ⅰ, Ⅱ and Ⅲ during processing, and obtain the best processing parameters, and can effectively distinguish the processed and unprocessed atractylodes, which can be optimized as processing conditions. The rapid detection tool provides a reference for the quality control of Chinese herbal medicines.
引文
[1]朱品松,房怀成,朱红光.七味白术散治疗小儿迁延性腹泻25例临床效果分析[J].中外医学研究,2017,15(2):128-129.
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[9]葛建,楼纪东,林芳,等.反相高效液相色谱法同时测定参苓白术颗粒中白术内酯Ⅱ和白术内酯Ⅲ的含量[J].时珍国医国药,2009,20(6):1319-1321.
[10] Chen Q,He H,Li P,et al. Identification and quantification of atractylenolide I and atractylenolideⅢin Rhizoma Atracty lodes Macrocephala by liquid chromatography-ion trap mass spectrometry[J]. Biomed Chromatogr,2013,27(6):699-707.
[11] Yan H,Sun Y,Zhang Q,et al. Simultaneous determination and pharmacokinetic study of Atractylenolide I,ⅡandⅢin rat plasma after intragastric administration of Baizhufuling extract and Atractylodis extract by UPLCMS/MS[J]. J Chromatogr B Analyt Technol Biomed Life Sci,2015, 993-994:86-92.
[12]钟艳梅,冯毅凡,郭姣.基于UPLC/Q-TOFMS技术的白术药材化学成分快速识别研究[J].质谱学报,2015,36(1):72-77.
[13]石晓,黄艳萍.GC-MS分析白术炮制前后化学成分的变化[J].食品与药品,2011,13(1):36-38.
[14] Chen Q,He H,Li P,et al. Identification and quantification of atractylenolide I and atractylenolideⅢin Rhizoma Atractylodes Macrocephala by liquid chromatography-ion trap mass spectrometry[J]. BMC,2013,27(6):699-707.
[15] Shi YY,Guan SH,Tang RN,et al. Simultaneous determination of atractylenolideⅡand atractylenolideⅢby liquid chromatography-tandem mass spectrometry in rat plasma and its application in a pharmacokinetic study after oral administration of Atractylodes macrocephala Rhizoma extract[J]. BMC,2012,26(11):1386-1392.
[16] Yao CM,Yang XW. Bioactivity-guided isolation of polyacetylenes with inhibitory activity against NO production in LPS-activated RAW264.7 macrophages from the rhizomes of Atractylodes macrocephala[J]. J Ethnopharmacol,2014,151(2):791-799.
[17] Huang H,Shi H,Feng S,et al. Quick detection of traditional Chinese medicine ‘Atractylodis Macrocephalae Rhizoma’ pieces by surface-enhanced Raman spectroscopy[J].Laser Phys,2013,23(1):015601-1-015601-4.
[18] Shambhunath Bose,Hojun Kim. Evaluation of in vitro anti-inflammatory activities and protective effect of fermented preparations of Rhizoma Atractylodis Macrocephalae on intestinal barrier function against lipopolysaccharide insult[J]. Evid Based Complement Alternat Med,2013,2013(4):363 076-363 091.
[19]蔡银燕,石婷婷,等.TLCS法测定白术炮制前后苍术酮的含量[J].中华中医药学刊,2012(3):515-516.
[20]陈鸿平.土炒白术健脾止泻作用增强的机制研究[D].成都:成都中医药大学,2011.
[21]李玲辉,窦德强.白术挥发油中苍术酮的稳定性研究[J].世界科学技术-中医药现代化,2014(1):193-198.
[22]李伟,文红梅,雀小兵,等.白术的炮制机理及其倍半萜成分转化的研究[J].中国中药杂志,2006,31(19):1600-1603.
[23]王小芳,王芳,张亚环,等.白术挥发油中苍术酮氧化反应的动力学[J].应用化学,2007,24(3):301-305.
[2]官国东,谭静,叶颖,等.半夏白术天麻汤加味治疗痰浊上扰证偏头痛临床疗效和治疗前后综合评分情况比较观察[J].中国医学创新,2016,13(7):80-83.
[3]赵秀静,李文茹.半夏白术天麻汤合桃红四物加减联合西药治疗缺血性中风的效果[J].中国医药导报,2016,13(33):157-160.
[4]陈一竹,杨文龙,郭玲玉,等.白术内酯Ⅱ抗血小板作用及对血小板中蛋白激酶B磷酸化水平的影响[J].中国医药导报,2016,13(11):18-21,26.
[5]周爱珍,王和平,程斌.白术的炮制机理研究进展[C].//现代化中药制剂发展与中药药理学研究交流会.2009.
[6]容穗华,林海,高妮.白术炮制工艺及炮制原理的研究[J].中国中药杂志,2011,36(8):1001-1003.
[7] Diao JH,Yang SQ,Liu S,et al. Study on HPLC fingerprint of Atractylodes japonica and analysis of the contents of atractylenolideⅠand atractylenolideⅢ[J]. China Pharmacy,2012,23(39):3714-3717.
[8] Liu Y,Cai Q. HPLC determination of atractylenolide and atractylenolide in 50 batches crude drugs and slices of Atractylodes macrocephala Koidz. from different sources[J].CJPA,2012,32(7):1249-1252.
[9]葛建,楼纪东,林芳,等.反相高效液相色谱法同时测定参苓白术颗粒中白术内酯Ⅱ和白术内酯Ⅲ的含量[J].时珍国医国药,2009,20(6):1319-1321.
[10] Chen Q,He H,Li P,et al. Identification and quantification of atractylenolide I and atractylenolideⅢin Rhizoma Atracty lodes Macrocephala by liquid chromatography-ion trap mass spectrometry[J]. Biomed Chromatogr,2013,27(6):699-707.
[11] Yan H,Sun Y,Zhang Q,et al. Simultaneous determination and pharmacokinetic study of Atractylenolide I,ⅡandⅢin rat plasma after intragastric administration of Baizhufuling extract and Atractylodis extract by UPLCMS/MS[J]. J Chromatogr B Analyt Technol Biomed Life Sci,2015, 993-994:86-92.
[12]钟艳梅,冯毅凡,郭姣.基于UPLC/Q-TOFMS技术的白术药材化学成分快速识别研究[J].质谱学报,2015,36(1):72-77.
[13]石晓,黄艳萍.GC-MS分析白术炮制前后化学成分的变化[J].食品与药品,2011,13(1):36-38.
[14] Chen Q,He H,Li P,et al. Identification and quantification of atractylenolide I and atractylenolideⅢin Rhizoma Atractylodes Macrocephala by liquid chromatography-ion trap mass spectrometry[J]. BMC,2013,27(6):699-707.
[15] Shi YY,Guan SH,Tang RN,et al. Simultaneous determination of atractylenolideⅡand atractylenolideⅢby liquid chromatography-tandem mass spectrometry in rat plasma and its application in a pharmacokinetic study after oral administration of Atractylodes macrocephala Rhizoma extract[J]. BMC,2012,26(11):1386-1392.
[16] Yao CM,Yang XW. Bioactivity-guided isolation of polyacetylenes with inhibitory activity against NO production in LPS-activated RAW264.7 macrophages from the rhizomes of Atractylodes macrocephala[J]. J Ethnopharmacol,2014,151(2):791-799.
[17] Huang H,Shi H,Feng S,et al. Quick detection of traditional Chinese medicine ‘Atractylodis Macrocephalae Rhizoma’ pieces by surface-enhanced Raman spectroscopy[J].Laser Phys,2013,23(1):015601-1-015601-4.
[18] Shambhunath Bose,Hojun Kim. Evaluation of in vitro anti-inflammatory activities and protective effect of fermented preparations of Rhizoma Atractylodis Macrocephalae on intestinal barrier function against lipopolysaccharide insult[J]. Evid Based Complement Alternat Med,2013,2013(4):363 076-363 091.
[19]蔡银燕,石婷婷,等.TLCS法测定白术炮制前后苍术酮的含量[J].中华中医药学刊,2012(3):515-516.
[20]陈鸿平.土炒白术健脾止泻作用增强的机制研究[D].成都:成都中医药大学,2011.
[21]李玲辉,窦德强.白术挥发油中苍术酮的稳定性研究[J].世界科学技术-中医药现代化,2014(1):193-198.
[22]李伟,文红梅,雀小兵,等.白术的炮制机理及其倍半萜成分转化的研究[J].中国中药杂志,2006,31(19):1600-1603.
[23]王小芳,王芳,张亚环,等.白术挥发油中苍术酮氧化反应的动力学[J].应用化学,2007,24(3):301-305.