铁牛七脂肪酸微波辅助提取及GC-MS分析研究
|
摘要
铁牛七(Aconitum szechenyianum Gay.)是毛莨科(Ranunculaceae)乌头属(Aconitum L)植物铁棒锤的干燥块根,主要分布于陕西秦岭山脉的太白山,生长于海拔2500米以上的山地草丛或林缘,是铁棒锤的别称。铁棒锤为陕、甘、宁、藏等地应用较广的一种民间草药,具有活血祛瘀,祛风湿,止痛,消肿败毒,去腐生肌,止血,治疗跌打损伤,风湿性关节炎,腰腿痛,劳伤,恶疮,痈肿,无名肿毒,冻疮,毒蛇咬伤等作用。药理学研究表明该药制成注射液有很强的镇痛、局麻、抑制呼吸、抗炎作用。关于铁牛七化学成分的研究已有报道,但尚未见到关于铁牛七脂肪酸研究的具体报道。
本论文包括文献综述和研究报告两部分内容。
第1章:文献综述
1.铁牛七研究概况
包括铁牛七概述、资源分布及鉴定、化学成分研究、药理作用的现状和进展等。
2.微波辅助提取研究概况
微波辅助提取研究概况部分涉及微波及其特性、微波加热的原理及特点、微波辅助提取法的原理及特点、微波辅助提取仪器及实验条件、微波辅助提取的应用实例几方面。
3.脂肪酸研究概况
包括脂肪酸的提取、脂肪酸的甲酯化、脂肪酸分析、脂肪酸的药理作用等方面内容。
第2章:研究报告
课题主要研究内容为:
1.微波辅助提取铁牛七脂肪酸
探讨了不同提取溶剂、溶剂浓度、微波提取功率、微波辐射时间以及料液比等条件对提取得率的影响。实验结果表明,铁牛七脂肪酸的最佳微波提取条件为:微波功率400W,溶剂丙酮浓度90%,料液比lg∶16 mL,微波辐射时间5min。最优条件下,铁牛七总脂肪酸提取率达13.0%。
2.铁牛七脂肪酸索氏提取
10.0g铁牛七药材粉末,用两张脱脂滤纸包起来装入索氏提取装置提取管内,加160mL90%丙酮于提取瓶内,连续回流提取6h。此条件下,铁牛七脂肪酸提取率为3.8%。
3气相色谱-质谱联用分析铁牛七脂肪酸成分
分别优化进样口温度、进样模式、分流比和进样量、载气流速、程序升温,建立最佳分析铁牛七脂肪酸成分的GC-MS条件。具体条件为:选择Rtx(?)-5MS%dipheny-95%dimethylpolysiloxane(0.25mm×30.0m,0.25μm)弹性石英毛细管色谱柱分析铁牛七提取物成分,程序升温为初温184℃,以0.2℃/min升温至191℃,进样口温度:260℃,分流进样模式,分流比:10:1,流速:1.00 mL/min,进样量:1μL;电子轰击(EI)离子源,离子源温度200℃,接口温度200℃,电子能量70eV,倍增器电压0.9kV,溶剂延迟时间4.5min,质量扫描范围m/z 40～500amu。
按照上述已建立好的GC-MS分析条件,铁牛七微波辅助提取和索氏提取两种方法的提取物经甲酯化衍生后,对其进行分离和分析,得到不同提取物各自总离子流色谱图(TIC)。各色谱峰相应的质谱图经人工解析及NIST05和NIST05s谱库检索,按各色谱峰的质谱碎片图与文献核对,查对有关质谱资料,对基峰、质荷比和相对丰度等方面进行直观比较,确定其化学成分,并用面积归一化法,测定出其相对含量。
4.铁牛七脂肪酸两种提取方法的比较
微波辅助提取物和索氏提取物分别鉴定出8,9种脂肪酸,所鉴定脂肪酸成分相似,主要是十四烷酸、十五烷酸、棕榈油酸、棕榈酸、十七烷酸、硬脂酸、亚油酸、亚麻酸、油酸,相同脂肪酸的相对含量略有差异。与传统索氏提取法时间6 h提取率3.8%相比,微波辅助提取时间大大缩短(仅是索氏提取的1/72),提取率却远高于索氏提取,且溶剂用量少,消耗能量少,CO_2排放量少对环境影响小。因此,微波辅助提取铁牛七脂肪酸具有产率高、时间短、能耗低等优点,较索氏提取优势明显。
Aconitum szechenyianum Gay. is dry earthnut of Ranunculaceae Plants Aconitum pendulum Busch., and it is mainly produced in Shannxi Taibai, growing in the mountainous grasscluster or forest edge of the elevation more than 2500 meters. Aconitum pendulum Busch. is mainly distributed in some regions of China, such as Xizang, Ningxia, Gansu, Shaanxi etc provinces . As a traditional Chinese medicinal herb, it exhibits blood-activated, detumescent and styptic effects, and treats joint pain, arthritic and rheumatic diseases etc. Pharmacological studies demonstrated that its injection possesses anti-inflammatory, analgesic and antitumor activities. There were a few reports on the constituents of Aconitum szechenyianum Gay., but to the best of our knowledge, no detailed report has yet appeared on the fatty acid components of it up to now.
There are two parts in this thesis:
Part one: Review
1. Study survey of Aconitum szechenyianum Gay.
It includes summary, resource distribution and authentication, study progress on chemical composition, pharmacological effects about Aconitum szechenyianum Gay.
2. Study survey of microwave-assisted extraction
It includes the definition and characteristics of microwave, the theory and characteristics of microwave heating and microwave-assisted extraction, the extraction apparatus, experiment condition and the application.
3. Study survey of fatty acids
It mainly involves extraction, derivatization to methyl esters, analysis and pharmacological research of fatty acids.
Part two: Research papers
Four main contents are included in this part.
1. Microwave-assisted extraction (MAE) of fatty acids from Aconitum szechenyianum Gay. The extraction solvent, solvent concentration, microwave power, radiation time, and ratio of solid to liquid were valued to compare the extraction yield of fatty acids. The optimum process condition was confirmed that microwave power was 400 W, acetone-water solvent concentration 90%, ratio of solid to liquid 1 g:16 mL, radiation time 5 min, and an extraction yield of 13.0% of total fatty acids could be obtained.
2. Soxhiet extraction (SE) of fatty acids from Aconitum szechenyianum Gay.
About 10.0 g powder was weighed, quantitatively transferred into a filter paper extraction thimble and inserted into a 250 mL reflux flask, then extracted with 160 mL 90% acetone-water solvent for about 6 h in a soxhiet apparatus.
3. Analysis of fatty acids in extracts of Aconitum szechenyianum Gay. with GC-MS
The analysis condition was optimized at the aspects of injection temperature, split mode, split ratio, injection volume, flow of carrier gas, temperature programmed and so on. The proper conditions are as follows: A fused silica capillary Rtx~(?)-5MS%dipheny-95% dimethylpolysiloxane column (30 m×0.25 mm i.d., film thickness 0.25μm) was used for the separation. Helium at a constant flow-rate of 1.00 mL/min was used as the carrier gas. 1μL extract was injected into the column with a split ratio set at 10:1 and injector port temperature at 260℃. The GC program was initiated by a column temperature set at 184℃, and then increased to 191℃at a rate of 0.2℃/min. Temperatures of the ion source and interface were all 200℃. The mass spectrometer was operated with El-mode at 70eV and the mass range was from m/z 40 to 500 amu.
The extracts of Aconitum szechenyianum Gay. obtained by microwave-assisted extraction and soxhiet extraction were identified respectively under the optimum GC-MS analysis condition. And relative amount of individual components were calculated based on GC peak areas.
4. Comparision of microwave-assisted extraction and soxhiet extraction
It can be seen that 8, 9 kinds of fatty acids in the MAE and SE extracts have been identified respectively. The chemical compositions of both extracts are similar, yet relative amount of the same fatty acids have few difference. The main components are palmitoleic acid, palmitic acid, linoleic acid, linolenic acid, oleic acid and stearic acids. Compared with soxhiet extraction, much shorter extraction time, better yield, lower cost and better environment ecology is advantageous for the proposed microwave-assisted extraction method.
本论文包括文献综述和研究报告两部分内容。
第1章:文献综述
1.铁牛七研究概况
包括铁牛七概述、资源分布及鉴定、化学成分研究、药理作用的现状和进展等。
2.微波辅助提取研究概况
微波辅助提取研究概况部分涉及微波及其特性、微波加热的原理及特点、微波辅助提取法的原理及特点、微波辅助提取仪器及实验条件、微波辅助提取的应用实例几方面。
3.脂肪酸研究概况
包括脂肪酸的提取、脂肪酸的甲酯化、脂肪酸分析、脂肪酸的药理作用等方面内容。
第2章:研究报告
课题主要研究内容为:
1.微波辅助提取铁牛七脂肪酸
探讨了不同提取溶剂、溶剂浓度、微波提取功率、微波辐射时间以及料液比等条件对提取得率的影响。实验结果表明,铁牛七脂肪酸的最佳微波提取条件为:微波功率400W,溶剂丙酮浓度90%,料液比lg∶16 mL,微波辐射时间5min。最优条件下,铁牛七总脂肪酸提取率达13.0%。
2.铁牛七脂肪酸索氏提取
10.0g铁牛七药材粉末,用两张脱脂滤纸包起来装入索氏提取装置提取管内,加160mL90%丙酮于提取瓶内,连续回流提取6h。此条件下,铁牛七脂肪酸提取率为3.8%。
3气相色谱-质谱联用分析铁牛七脂肪酸成分
分别优化进样口温度、进样模式、分流比和进样量、载气流速、程序升温,建立最佳分析铁牛七脂肪酸成分的GC-MS条件。具体条件为:选择Rtx(?)-5MS%dipheny-95%dimethylpolysiloxane(0.25mm×30.0m,0.25μm)弹性石英毛细管色谱柱分析铁牛七提取物成分,程序升温为初温184℃,以0.2℃/min升温至191℃,进样口温度:260℃,分流进样模式,分流比:10:1,流速:1.00 mL/min,进样量:1μL;电子轰击(EI)离子源,离子源温度200℃,接口温度200℃,电子能量70eV,倍增器电压0.9kV,溶剂延迟时间4.5min,质量扫描范围m/z 40～500amu。
按照上述已建立好的GC-MS分析条件,铁牛七微波辅助提取和索氏提取两种方法的提取物经甲酯化衍生后,对其进行分离和分析,得到不同提取物各自总离子流色谱图(TIC)。各色谱峰相应的质谱图经人工解析及NIST05和NIST05s谱库检索,按各色谱峰的质谱碎片图与文献核对,查对有关质谱资料,对基峰、质荷比和相对丰度等方面进行直观比较,确定其化学成分,并用面积归一化法,测定出其相对含量。
4.铁牛七脂肪酸两种提取方法的比较
微波辅助提取物和索氏提取物分别鉴定出8,9种脂肪酸,所鉴定脂肪酸成分相似,主要是十四烷酸、十五烷酸、棕榈油酸、棕榈酸、十七烷酸、硬脂酸、亚油酸、亚麻酸、油酸,相同脂肪酸的相对含量略有差异。与传统索氏提取法时间6 h提取率3.8%相比,微波辅助提取时间大大缩短(仅是索氏提取的1/72),提取率却远高于索氏提取,且溶剂用量少,消耗能量少,CO_2排放量少对环境影响小。因此,微波辅助提取铁牛七脂肪酸具有产率高、时间短、能耗低等优点,较索氏提取优势明显。
Aconitum szechenyianum Gay. is dry earthnut of Ranunculaceae Plants Aconitum pendulum Busch., and it is mainly produced in Shannxi Taibai, growing in the mountainous grasscluster or forest edge of the elevation more than 2500 meters. Aconitum pendulum Busch. is mainly distributed in some regions of China, such as Xizang, Ningxia, Gansu, Shaanxi etc provinces . As a traditional Chinese medicinal herb, it exhibits blood-activated, detumescent and styptic effects, and treats joint pain, arthritic and rheumatic diseases etc. Pharmacological studies demonstrated that its injection possesses anti-inflammatory, analgesic and antitumor activities. There were a few reports on the constituents of Aconitum szechenyianum Gay., but to the best of our knowledge, no detailed report has yet appeared on the fatty acid components of it up to now.
There are two parts in this thesis:
Part one: Review
1. Study survey of Aconitum szechenyianum Gay.
It includes summary, resource distribution and authentication, study progress on chemical composition, pharmacological effects about Aconitum szechenyianum Gay.
2. Study survey of microwave-assisted extraction
It includes the definition and characteristics of microwave, the theory and characteristics of microwave heating and microwave-assisted extraction, the extraction apparatus, experiment condition and the application.
3. Study survey of fatty acids
It mainly involves extraction, derivatization to methyl esters, analysis and pharmacological research of fatty acids.
Part two: Research papers
Four main contents are included in this part.
1. Microwave-assisted extraction (MAE) of fatty acids from Aconitum szechenyianum Gay. The extraction solvent, solvent concentration, microwave power, radiation time, and ratio of solid to liquid were valued to compare the extraction yield of fatty acids. The optimum process condition was confirmed that microwave power was 400 W, acetone-water solvent concentration 90%, ratio of solid to liquid 1 g:16 mL, radiation time 5 min, and an extraction yield of 13.0% of total fatty acids could be obtained.
2. Soxhiet extraction (SE) of fatty acids from Aconitum szechenyianum Gay.
About 10.0 g powder was weighed, quantitatively transferred into a filter paper extraction thimble and inserted into a 250 mL reflux flask, then extracted with 160 mL 90% acetone-water solvent for about 6 h in a soxhiet apparatus.
3. Analysis of fatty acids in extracts of Aconitum szechenyianum Gay. with GC-MS
The analysis condition was optimized at the aspects of injection temperature, split mode, split ratio, injection volume, flow of carrier gas, temperature programmed and so on. The proper conditions are as follows: A fused silica capillary Rtx~(?)-5MS%dipheny-95% dimethylpolysiloxane column (30 m×0.25 mm i.d., film thickness 0.25μm) was used for the separation. Helium at a constant flow-rate of 1.00 mL/min was used as the carrier gas. 1μL extract was injected into the column with a split ratio set at 10:1 and injector port temperature at 260℃. The GC program was initiated by a column temperature set at 184℃, and then increased to 191℃at a rate of 0.2℃/min. Temperatures of the ion source and interface were all 200℃. The mass spectrometer was operated with El-mode at 70eV and the mass range was from m/z 40 to 500 amu.
The extracts of Aconitum szechenyianum Gay. obtained by microwave-assisted extraction and soxhiet extraction were identified respectively under the optimum GC-MS analysis condition. And relative amount of individual components were calculated based on GC peak areas.
4. Comparision of microwave-assisted extraction and soxhiet extraction
It can be seen that 8, 9 kinds of fatty acids in the MAE and SE extracts have been identified respectively. The chemical compositions of both extracts are similar, yet relative amount of the same fatty acids have few difference. The main components are palmitoleic acid, palmitic acid, linoleic acid, linolenic acid, oleic acid and stearic acids. Compared with soxhiet extraction, much shorter extraction time, better yield, lower cost and better environment ecology is advantageous for the proposed microwave-assisted extraction method.
引文
[1]冉先德.中华药海[M].哈尔滨:哈尔滨出版社,1993:1467-1480.
[2]高渌纹.有毒中药临床精要[M].北京:学苑出版社,2000:28.
[3]胡本祥,李华,王宇鹏,闫平川.铁棒锤的显微鉴别[J].西北药学杂志,2004,19(1):17-19.
[4]杨智锋,刘建峰,张红,党秋萍,郑洁.铁棒锤药材质量标准研究[J].中国中药杂志,2005,30(22):1771-1773.
[5]陈凤娥.铁棒锤的研究进展[J].安徽农业科学,2007,35(32):10353,10360.
[6]胡本祥,李华,王宇鹏,闫平川.铁棒锤的生药研究[J].中国中医药信息杂志,2003,9(10):20-21.
[7]朱子清,程东亮,常贵桃,刘玉卿.伏毛铁棒锤生物碱的研究[J].兰州大学学报:自然科学版,1980,10(3):26-28.
[8]张帆,王兴明,彭树林,丁立生.伏毛铁棒锤根部二萜生物碱的研究[J].中国药学杂志,2006,41(24):1851-1854.
[9]孙文基,沙振方,王艾兴,赵晓文,袁忠智.铁棒锤化学成分研究[J].药学学报,1989,24(1):71-74.
[10]李洪刚,杨建萍,田义杰,赵毅军.伏毛铁棒锤地上部分生物碱成分研究[J].中草药,1997,28(5):265-266.
[11]符华林.我国乌头属药用植物的研究概况[J].中药材,2004,27(2):149-152.
[12]沈映君.中药药理学[M].北京:人民卫生出版社,2000:382,490.
[13]宋东江,陆满文,彭建中.乌头碱类化合物抗炎作用研究进展[J].中草药,1990,21(11):43-45.
[14]胡学军,钟燕珠.乌头类中药及其制剂的镇痛作用[J].中医药研究,2001,17(4):56-58.
[15]宋东江,陆满文.去氧乌头碱的抗炎、镇痛和解热作用[J].中国药理学通报,1987,(3):157-161.
[16]郭晓庄.有毒中草药大辞典[M].天津:天津科技翻泽出版公司,1992:434-440.
[17]中华人民共和国卫生部药政管理局,等.现代实用本草(上册)[M].北京:人民卫生出版社,1997:75-79,496-502,519-525.
[18]王雅贤,贾宽,张德山,王桂山.乌头碱对小鼠免疫功能影响的实验研究[J].中 医药信息,1989,(5):40-41.
[19]段泾云,刘小平,李秦.铁牛七抗肿瘤作用的实验研究[J].深圳中医结合杂志,1998,8(1):13-15.
[20]徐秀丽,杨继维.内服铁棒锤药酒中毒2例[J].西北药学志,1995,10(4):188.
[21]姜希才,刘燕飞,吴湘华.含乌头碱类中药中毒的中毒表现及其解救[J].中国乡村医生杂志,2000,19(1):4-5.
[22]王晓燕.中草药“铁棒锤”中毒致频发性多形型室性早搏1例[J].陕西中医学院学报,2000,23(6):39.
[23]郭维图.微波技术在中药提取研发与生产中的应用[J].医药工程设计,2006,27(6):50-58.
[24]K.Ganzler,A.Salg6,K.Valk6.Microwave Extraction:A Novel Sample Preparation Method for Chromatography[J].Journal of Chromatography A,1986,371(1):299-306.
[25]谢永荣,腾莉丽,余月容.微波法提取柑桔皮中天然色素[J].赣南师范学院学报,1994,(2):34-37.
[26]梅成.微波萃取技术的应用[J].中成药,2002,24(2):134-135.
[27]A.Zlotoraynski.The Application of Microwave Radiation to Aalytical and Environmental Chemistry[J].Critical Reviews in Analytical Chemistry,1995,(1):43.76.
[28]王艳,张铁军.微波萃取技术在中药有效成分提取中的应用[J].中草药,2005,36(3):470-473.
[29]M.E.Lucchesi,E Chemat,J.Smadja.Solvent-free Microwave Extraction of Essential Oil from Aromatic Herbs:Comparison with Conventional Hydro-distillation[J].Journal of Chromatography A,2004,1043(2):323-327.
[30]M.E.Lucchesi,F.Chemat,J.Smadja.An Original Solvent Free Microwave Extraction of Essential Oils from Spices[J].Flavour and Fragrance Journal,2004,19(2):134-138.
[31]张代佳,刘传斌,修志龙,昌增益.微波技术在植物胞内有效成分提取中的应用[J].中草药,2000,31(9):附5-6.
[32]J.R.J.Pare,M.Sigouin,J.Lapointe.Microwave-assisted Natural Products Extraction.1991,US Ptaent No.519588(5002784).
[33]J.R.J.Pare,J.M.R.Belnager,S.S.Stafford.Microwave-assisted Process (MAP~(TM)):A New Tool for the Analytical Laboratory[J].TrAC Trends in Analytical Chemistry,1994,13(4):176-184.
[34]D.R.Bgauhrst,D.M.P.Mingos.Design and Application of a Relfux Modification for the Synthesis of Organmetallic Compounds Using Microwave Dielectric Loss Hetaing Effects[J].Journal of Organometallic Chemistry,1990,384(3):C57-C60.
[35]D.R.Baghurst,S.R.Cooper,D.L.Greene,D.M.P.Mingos,S.M.Reynolds.Applictaion of Microwave Dielectric Loss Heating Effects for the Rapid and Convenient Synthesis of Coordination Compounds[J].Polyhedron,1990,9(6):893-895.
[36]冯年平,沈岚,韩朝阳,朱沪平,范广平.决明子微波萃取法与常用提取方法的比较[J].中成药,2004,26(3):189-191.
[37]李核,李攻科,张展霞.密闭系统中微波辅助萃取机制探讨[J].分析测试学报,2004,32(5):12-16.
[38]李核,李攻科,张展霞.影响微波辅助萃取虎杖中白黎芦醇产率的一些重要操作参数[J].分析化学,2003,31(11):1341-1344.
[39]李核,李攻科,张展霞.密闭式微波系统的微波辅助萃取动力学模型[J].中山大学学报(自然科学版),2004,43(3):40-44.
[40]符嫦娥,韩伟.微波萃取技术[J].化工技术与开发,2004,3(1):22-52.
[41]C.W.Huie.A Review of Modem Sample PerPartaion Techniques for the Extrctaion and Analysis of Medicine Plant[J].Bioanaltyical Chemisrty,2002,373(1-2):23-30.
[42]段胜林.微波辐射技术在食品萃取工业和化学工业上的应用[J].食品工业科技,1999,20(2):70-71.
[43]郝金玉,韩伟,邓修.新鲜银杏叶经微波辅助提取后微观结构的变化[J].中草药,2002,33(8):739-741.
[44]韩伟,高姗,邓修.微波辐射促进阔叶十大功劳叶萃取过程的研究[J].华东理工大学学报,2002,28(4):337-340.
[45]王娟,沈平攘,沈永嘉.微波辅助萃取葛根和刺五加微观机制的研究[J].中草药,2002,35(1):31-33.
[46]S.Chemat,H.Ant-Amar,A.Lagha,D.C.Esveld.Microwave-assisted Extraction Kinetics of Terpenes from Caraway Seeds[J].Chemical Engineering and Porcessing,2005,44(12):1320-1326.[47]沈岚,冯年平,韩朝阳.微波萃取对不同形态结构中药及含不同极性成分中药的选择性研究[J].中草药,2002,33(7):604-607. [48]王志祥,李红娟,万水昌,李菊,乐龙.微波萃取技术及其在中药有效成分提取中的应用[J].时珍国医国药,2007,18(5):1245-1247. [49]栾伟.石蒜中加兰他敏的微波辅助提取、分离和分析的研究[D].广州:中山大学,2004. [50]冯年平,范广平,吴春兰,韩朝阳.微波萃取技术在中药提取中的应用[J].世界科技技术-中药现代化
药物生产技术,2002,4(2):49-53. [51]刘川生,王平,王立飞,梅成,陈薇薇.微波萃取技术在天然药物提取中的研究进展[J].中国天然药物,2003,1(3):187-192. [52]郝金玉,韩伟,周永伟,刘海峰,邓修.微波萃取器内流体的沉降速度分布[J].化学工业与工程,2002,19(5):343-348. [53]Z.C.Kodba,J.Marsel.Microwave-assisted Extraction and Sonication of Polychlorobiphenils from River Sediments and Risk Assessment by Toxic Equivalency Factors[J].Chromatographia,1999,49(1-2):21-27. [54]J.C.Young.Microwave-assisted Extraction of the Fungal Metabolite Ergosterol and Total Fatty Acids[J].Journal of Agriculture and Food Chemistry,1995,43(11):2904-2910. [55][55]I.R.Pereiro,A.Wasik,R.Lobinski.Determination of Mercury Species in Fish Rreference Materials by Isothermal Multicapillary Gas Chromatography with Atomic Emission Detection after Microwave-assisted Solubilization and Solvent Extraction[J].Journal of Analytical Atomic Spectrometry,1998,13(8):743-747. [56]M.E.Lucchesi,F.Chemat,J.Smadja.An Original Solvent Free Microwave Extraction of Essential Oils from Spices[J].Flavour and Fragrance Journal,2004,19(2):134-138. [57]A.Pastor,E.Vázquez,R.Ciscar,M.de la Guardia.Efficiency of the Microwave-assisted Extraction of Hydrocarbons and Pesticides from Sediments [J].Analytica Chimica Acta,1997,344(3):241-249. [58]C.S.Eskilsson,E.Bj6rklund.Analytical-scale Microwave-assisted Extraction[J].Journal of Chromatography A,2000,902(1):227-250. [59]H.M.J.Pylypiw,T.L.Arsenault,C.M.Thetford,M.M.J.Incorvia.Suitability of Microwave-assisted Extraction for Multiresidue Pesticide Analysis of Produce [J].Journal of Agriculture and Food Chemistry,1997,45(9):3522-3528.
[60]M.P.Llompart,R.A.Lorenzo,R.Cela,K.Li,J.M.R.Belanger,J.R.J.Paré.Evaluation of SupercriticaI Fluid Extraction,Microwave-assisted Extraction and Sonication in the Determination of Some Phenolic Compounds from Various Soil Matrices[J].Journal of Chromatography A,1997,774(1-2):243-251.
[61]邓湘庆,龚盛昭.微波辅助萃取中药有效成分的研究进展[J].广东化工,2006,33(12):89-92.
[62]I.J.Barnabas,J.R.Dean,I.A.Fowlis,S.P.Owen.Extraction of Polycyclic Aromatic Hydrocarbons from Highly Contaminated Soils Using Microwave Energy[J].Analyst,1995,120:1897-1904.
[63]元英进,刘明言,董岸杰.中药现代化生产关键技术[M].北京:化学工业出版社,2002.
[64]C.Molins,E.A.Hogendoom,E.Dijkman,H.A.G.Heusinkveld,R.A.Baumann.Determination of Linuron and Related Compounds in Soil by Microwave-assisted Solvent Extraction and Reversed-phase Liquid Chromatography with UV Detection[J].Journal of Chromatography A,2000,869(1-2):487-496.
[65]M.Letellier,H.Budzinski.Influence of Sediment Grain Size on the Efficiency of Focused Microwave Extraction of Polycyclic Aromatic Hydrocarbons[J].Analyst,1999,124(1):5-14.
[66]J.A.Maria,M.R.B.Jacqueline,E C.Padilla,J.R.J.Paré.Influence of Solvent,Matrix Dielectric Properties,and Applied Power on the Liquid-phase Microwave-assisted Processes(MAP~(TM)) Extraction of Ginger[J].Food Research International,2003,36(5):499-504.
[67]孔臻,刘钟栋.微波法从苹果渣中提取果胶的研究[J].郑州粮食学报,2000,21(2):11-15.
[68]唐小俊,张名位,池建伟,张雁,施英,何焕清,张瑞芬.姬松茸多糖的微波辅助提取与含量测定[J].中国食品学报,2006,6(1):267-272.
[69]聂金媛,吴成岩,吴世容,李志良,微波辅助提取茯苓中茯苓多糖的研究[J].中草药,2004,35(12):1346-1348.
[70]黄璞,谢明勇,聂少平,陈奕,李昌,谢建华.响应曲面法优化微波辅助提取黑灵芝孢子多糖工艺研究[J].食品科学,2007,28(10):200-203.
[71]滑艳,邓雁如,汪汉卿.各种挥发油的药理活性及在医学方面的应用[J].天 然产物研究与开发,2003,15(5):467-470.
[72]Pare J R Jocelyn.1994,US5338557:Microwave Extraction of Volatile Oils.
[73]Pare J R Jocelyn.1995,US5458897:Microwave-assisted Extraction from Materials containing Organic Matter.
[74]Pare J R Jocelyn.1995,US5377426:Microwave-assisted Generation of Volatiles,of Supercritical Fluid,and Apparatus therefore.
[75]Pare J R Jocelyn.1996,US19947:Microwave-assisted Generation of Volatiles,of Supercritical Fluid,and Apparatus therefore.
[76]陈业高,海丽娜,毕先钧.微波辐射在天然药用活性成分提取分离中的应用[J].微波学报,2003,19(2):85-89.
[77]回瑞华,侯冬岩,李铁纯,关崇新.苦杏仁挥发油化学成分的微波-一时蒸馏萃取GC-MS分析[J].分析测试学报,2003,22(1):55-57.
[78]回瑞华,侯冬岩,李铁纯.微波-萃取木香挥发性化学成分的气相色谱-质谱分析[J].质谱学报,2003,24(4):471-476.
[79]回瑞华,侯冬岩,朱永强,刘晓媛.微波-同时蒸馏萃取分离肉桂挥发性成分分析[J].理化检验-化学分册,2006,42(2):105-108.
[80]赵金尧,陈春保,杨辉.赤芍及其相关药对中挥发油成分的研究[J].广州化学,2005,30(3):35-38.
[81]成玉怀,闰豫君,鲁建江.红景天叶中挥发油的微波提取初步实验[J].广东药学,2002,12(6):21-22.
[82]鲁建江,王莉,陈宏伟,孙萍.佩兰中挥发油的微波提取法[J].时珍国医国药,2001,12(9):774.
[83]谭仁祥.植物成分分析[M].北京:科学出版社.2000:386-413.
[84]高锦明.植物化学[M].北京:科学出版社,2003:217-254.
[85]M.Gao,W.Huang,M.RoyChowdhury,C.Z.Liu.Microwave-assisted Extraction of Scutellarin from Erigeron breviscapus Hand-Mazz and its Determination by High-performance Liquid Chromatography[J].Analytica Chimica Acta,2007,591(2):161-166.
[86]J.Y.Hao,W.Han,S.D.Huang,B.Y.Xue,X.Deng.Microwave-assisted Extraction of Artemisinin from Artemisia annua L[J].Separation and Purification Technology,2002,28(3):191-196.
[87]X.J.Pan,G.G.Niu,H.Z.Liu.Microwave-assisted Extraction of Tanshinones from Salvia miltiorrhiza bunge with Analysis by High-performance Liquid Chromatography[J].Journal of Chromatography A,2001,922(1-2):371-375.
[88]邹晓军,高小利.丹参中丹参素和原儿茶醛的微波提取工艺研究[J].中药材,2007,30(6):735-737.
[89]王楠.皂苷生物活性的研究进展[J].医学研究生学报,2007,20(2):211-214.
[90]刘永练,郑成,毛桃嫣,张新强,骆间仪.微波提取人参中活性成分人参皂苷的研究[J].广州大学学报(自然科学版),2006,5(6):52-55.
[91]Z.Y.Hu,M.Cai,H.H.Liang.Desirability Function Approach for the Optimization of Microwave-assisted Extraction of Saikosaponins from Radix Bupleuri[J].Separation and Purification Technology,2007,61:266-275.
[92]黎海彬.罗汉果皂苷的微波提取[J].食品科学,2007,28(3):143-147.
[93]程红霞,林强,程维明.苄基异喹啉类生物碱药理作用及机制的研究进展[J].中国新药与临床杂志,2006,25(5):392-397.
[94]刘覃,陈晓青,蒋新宇,吴升德.微波辅助提取龙葵中总生物碱的研究[J].天然产物研究与开发,2005,17(1):65-69.
[95]肖桂青,田云,卢向阳,方俊.微波辅助提取荷叶生物碱条件的优化[J].氨基酸和生物资源,2007,29(2):76-79.
[96]A.Brachet,P.Christten,J.I.Veuthcy.Focused Microwave-assisted Extraction of Cocaine and Benzoylecgonine from Coca Leaves[J].Phytochemical Analysis,2002,13(3):162-169.
[97]F.Zhang,B.Chen,S.Xiao,S.Z.Yao.Optimization and Comparison of Different Extraction Techniques for Sanguinarine and Chelerythrine in Fruits of Macleaya cordata(Willd) R.Br[J].Separation and Purification Technology,2005,42(3):283-290.
[98]江纪武.植物药有效成分手册[M].北京:人民卫生出版社,1986:3.
[99]李开泉,陈武,熊筱娟,王雪.乌索酸的化学、药理及临床应用进展[J].中成药,2002,24(9):709-711.
[100]L.Liu,W.R.Hudgins,S.Shack,M.Q.Yin,D.Samid.Cinnamic Acid:A Natural Product with Potential Use in Cancer Intervention[J].International Journal of Cancer,1995,62(3):345-350.
[101]王立新,韩广轩.齐墩果酸的化学及药理研究[J].药学实践杂志,2001,19(2):104-107.
[102]田瑛,董俊兴.天然产物中抗爱滋病病毒活性成分的研究进展[J].中国药学杂志,2002,37(6):401-406.
[103]郭锦棠,杨俊红,李雄勇,褚治德.微波与索氏提取甘草酸的正交买验研究[J].中国药学杂志,2002,37(12):919-922.
[104]孙秀利,秦培勇,谭天伟.微波法提取丹参中丹酚酸B的研究[J].中草药,2007,38(3):379-382.
[105]肖诗明,张忠,李勇,曾继光.苦荞麦麸皮中黄酮的提取工艺条件研究[J].食品科学,2006,27(1):156-158.
[106]张胜帮,赵玲玲.黄酮类化合物的提取纯化研究进展[J].温州大学学报·自然科学版,2007,28(5):25-29.
[107]陈斌,南庆贤,吕玲,周熙成.微波萃取葛根总异黄铜的工艺研究[J].农业工程学报,2001,17(6):123-126.
[108]Z.K.Guo,Q.H.Jin,G.Q.Fan,Y.P.Duan,C.Qin,M.J.Wen.Microwave-assisted Extraction of Effective Constituents from a Chinese Herbal Medicine Radix puerariae[J].Analytica Chimica Acta,2001,436(1):41-47.
[109]赵二劳,盖青青,张海容.微波萃取沙棘黄酮的研究[J].食品工业与发酵,2004,30(12):148-150
[110]朱蕾,王竹天,杨大进.葸醌类化合物的定性定量方法研究进展[J].中国食品卫生杂志,2006,18(2):155-158.
[111]吴拥军,孔娜,石杰,于斐,张洪权.中药巴戟天中蒽醌的提取与测定[J].安阳师范学院学报,2006(5):90-93.
[112]沈岚,冯年平,韩朝阳,朱沪平,范广平.大黄微波萃取法与常用提取方法的比较研究[J].中成药,2003,25(8):614-616.
[113]郝守祝,张虹,刘丽,李智恩,徐祖洪.微波技术在大黄游离蒽醌浸提中的应用[J].中草药,2002,33(1):23-26.
[114]张越华,曾和平.脂肪酸在生命过程中的作用研究进展[J].中国油脂,2006,31(12):11-16.
[115]马立红,王晓梅.多不饱和脂肪酸药理作用研究[J].吉林中医药,2006,26(12):69-70.
[116]李林强,李建科,刘迎利.超声波处理提取华山松籽油的研究[J].西北农林科技大学学报(自然科学版),2003,31(5):115-117.
[117]符嫦娥.微波萃取绿藻花生四烯酸及其纯化研究[M].华东理工大学硕士论文,20050120.
[118]范文洵.a-亚麻酸及其代谢产物EPA和DHA[J].生理科学进展,1988,19(2):110-113.
[119]邱磊.多不饱和脂肪酸的药理研究进展[J].药学实践杂志,1996,14(2):77-80.
[120]范亚苇,邓泽元,余永红,邓胜国,李静.不同脂肪酸甲酯化方法对共轭亚油酸分析的影响[J].中国油脂,2007,32(1):52-55.
[121]张亚刚,樊莉,文彬,马莉,吾满江·艾力.紫外可见分光光度法在共轭亚油酸定量分析中的应用[J].疆石油学院学报,2002,14(2):59-63.
[122]M.S.Manku.Analysis of γ-linolenic[J].Journal of Chromatographic Science,1983,8:1-11.
[123]Le-Ellen Dayhuff,Martha J.M.Wells.Identification of Fatty Acids in Fishes Collected from the Ohio River Using Gas Chromatography - Mass Spectrometry in Chemical Ionization and Electron Impact Modes[J].Journal of Chromatography A,2005,1098(1-2):144-149.
[124]徐秀兰,胡磊军,吴梧桐.脂肪酸的分析方法研究[J].药物生物技术,1998,5(3):161-165.
[125]郑立立,王磊,江克铮.鱼油中二十碳五烯酸和二十二碳六烯酸的气相色谱-红外光谱分析[J].分析化学,1994,2(4):383-385.
[126]赵先恩,索有瑞,王凌云,尤进茂.深海鱼油中脂肪酸的柱前衍生-高效液相色谱串联质谱分析[J].食品科学,2007,28(8):358-362.
[127]任其龙,熊任天,王宪达,吴平东.超临界流体色谱法分离二十碳五烯酸和二十二碳六烯酸[J].分析化学,2001,29(9):1076-1078.
[128]Tomá(?) Rezanka.Analysis of Polyunsaturated Fatty Acids Using High Performance Liquid Chromatography-Atmospheric Pressure Chemical Ionization Mass Spectrometry[J].Journal of High Resolution Chromatography,2000,23(4):338-342.
[129]T.K.Miwa,K.L.Mikolajczak,F.R.Earle,I.A.Wolff.Gas Chromatographic Characterization of Fatty Acids,Identification Constants for Mono- and Dicarboxylic Methyl Esters[J].Analticaly Chemistry,1960,32(13):1739-1742.
[130]徐学兵等.油脂化学[M].北京:中国商业出版社,1993:259-260.
[131]徐秀兰,胡磊军,吴梧桐.脂肪酸的分析方法研究[J].药物生物技术,1998,5(3):161-165.
[132]万新祥,张立.鱼油的药用价值[J].中国药学杂志,1990,25(7):392.
[133]C.D.Bannon,J.D.Craske,D.L.Felder,I.J.Garland,L.M.Norman.Analysis of Fatty Acid Methyl Esters with High Accuracy and Reliability:Ⅵ.Rapid Analysis by Split Injection Capillary Gas-Liquid Chromatography[J].Journal of Chromatography A,1987,407:231-241.
[134]D.E.Albertyn,C.D.Bannon,J.D.Craskeetal.Analysis of Fatty Acid Methyl Esters[J].Chromatographia,1982,247(3):71-74.
[135]K.Eder.Gas Chromatographic Analysis of Fatty Acid Methyl Esters[J].Journal of Chromatography B,1995,671(1-2):113-131.
[136]回瑞华,侯冬岩,李铁纯,李学成,刘晓媛,雷磊,国艳秋.食用植物油中脂肪酸的分析[J].鞍山师范学院学报,2006,8(6):19-21.
[137]邱磊,姜远英.多不饱和脂肪酸的药理研究进展[J].药学实志,1996,14(2):77-80.
[138]窦学廉,康毅.X-3多不饱和脂肪酸的药理研究进展[J].天津医科大学学报,1996,2(4):82-83.
[139]张金廷.脂肪酸及其深加工手册[M].北京:化工出版社,2002,8:362-363.
[140]张施军,朱薇,许颂.HP 4890D气相色谱仪在海豹油功效成分测定中的应用[J].水产科技情报,2000,27(2):169-171.
[141]曾惠玲.中药化学成分提取新技术研究进展[J].海峡药学,2005,17(5):1-3.
[142]王昌利,李君.中药有效成分提取方法研究进展[J].陕西中医函授,1995,(3):23-25.
[143]王昌利,范少敏.中药有效群体及有效成分提取分离方法研究进展[J].陕西中医学院学报,2001,24(6):60-62.
[144]李真,贾亮,贾绍义.中药有效成分提取技术及其应用[J].化学工业与工程,2005,22(6):450-455.
[145]李继遥,周学东,戴朝政,张萍.气相色谱及气相色谱-质谱联用技术分析牙菌斑脂肪酸方法的建立[J].华西口腔医学杂志,2000,18(6):386-388.
[146]李萍,刘丽芳.常用中药液相与气相色谱鉴定[M].北京:化学工业出版社,2005:19-20.
[147]张海松.中药猫爪草中挥发油和脂肪酸的气相色谱质谱联用分析[D].西安:陕西师范大学,2006。
[148]S.R.Heller,F.W.Melafferty,D.B.Stauffer,et al.GWA.EPA/NIH Mass Spectral Data Kase[M].Washington:US Government printing office,1978.
[149]丛浦珠.质谱学在天然有机化学中的应用[M].北京:科学出版社,1987.
[150]Y.Masada.Analysis of Essential Oils by Gas Chromatography and Mass Spectrometry[M].New York:John wile and sons.Inc.1976.
[151]张利,纪军,朱晓旺,吴圆圆,于环,张槟,李雪岭,孙喜琢.软脂酸诱导人肝癌HepG2细胞的凋亡[J].中国医学科学院学报,2004,26(6):671-676
[152]N.Fukuda,T.Etoh,K.Wada,et al.Differential Effects of Geometrical Isomers of Octadecadienoic Acids on Ketogenesis and Lipid Secretion in the Livers from Rats Fed a Cholesterol-enriched Diet[J].Annals of Nutrition and Metabolism,1995,39:185-192.
[153]李丕高,李西安,曹庆生.紫茉莉籽油的提取及其脂肪酸组成分析[J].中国油脂,2007,32(6):35-37
[154]余纲哲.鳗骨油的提取与分析[J].食品工业科技,1994,(3):66-69.
[155]汪茂田,谢培山,王忠东等编著.天然有机化合物提取分离与结构鉴定[M].化学工业出版社,2004:5.
[156]J.Bernard,Sciences et vie.2001,214:68.
[2]高渌纹.有毒中药临床精要[M].北京:学苑出版社,2000:28.
[3]胡本祥,李华,王宇鹏,闫平川.铁棒锤的显微鉴别[J].西北药学杂志,2004,19(1):17-19.
[4]杨智锋,刘建峰,张红,党秋萍,郑洁.铁棒锤药材质量标准研究[J].中国中药杂志,2005,30(22):1771-1773.
[5]陈凤娥.铁棒锤的研究进展[J].安徽农业科学,2007,35(32):10353,10360.
[6]胡本祥,李华,王宇鹏,闫平川.铁棒锤的生药研究[J].中国中医药信息杂志,2003,9(10):20-21.
[7]朱子清,程东亮,常贵桃,刘玉卿.伏毛铁棒锤生物碱的研究[J].兰州大学学报:自然科学版,1980,10(3):26-28.
[8]张帆,王兴明,彭树林,丁立生.伏毛铁棒锤根部二萜生物碱的研究[J].中国药学杂志,2006,41(24):1851-1854.
[9]孙文基,沙振方,王艾兴,赵晓文,袁忠智.铁棒锤化学成分研究[J].药学学报,1989,24(1):71-74.
[10]李洪刚,杨建萍,田义杰,赵毅军.伏毛铁棒锤地上部分生物碱成分研究[J].中草药,1997,28(5):265-266.
[11]符华林.我国乌头属药用植物的研究概况[J].中药材,2004,27(2):149-152.
[12]沈映君.中药药理学[M].北京:人民卫生出版社,2000:382,490.
[13]宋东江,陆满文,彭建中.乌头碱类化合物抗炎作用研究进展[J].中草药,1990,21(11):43-45.
[14]胡学军,钟燕珠.乌头类中药及其制剂的镇痛作用[J].中医药研究,2001,17(4):56-58.
[15]宋东江,陆满文.去氧乌头碱的抗炎、镇痛和解热作用[J].中国药理学通报,1987,(3):157-161.
[16]郭晓庄.有毒中草药大辞典[M].天津:天津科技翻泽出版公司,1992:434-440.
[17]中华人民共和国卫生部药政管理局,等.现代实用本草(上册)[M].北京:人民卫生出版社,1997:75-79,496-502,519-525.
[18]王雅贤,贾宽,张德山,王桂山.乌头碱对小鼠免疫功能影响的实验研究[J].中 医药信息,1989,(5):40-41.
[19]段泾云,刘小平,李秦.铁牛七抗肿瘤作用的实验研究[J].深圳中医结合杂志,1998,8(1):13-15.
[20]徐秀丽,杨继维.内服铁棒锤药酒中毒2例[J].西北药学志,1995,10(4):188.
[21]姜希才,刘燕飞,吴湘华.含乌头碱类中药中毒的中毒表现及其解救[J].中国乡村医生杂志,2000,19(1):4-5.
[22]王晓燕.中草药“铁棒锤”中毒致频发性多形型室性早搏1例[J].陕西中医学院学报,2000,23(6):39.
[23]郭维图.微波技术在中药提取研发与生产中的应用[J].医药工程设计,2006,27(6):50-58.
[24]K.Ganzler,A.Salg6,K.Valk6.Microwave Extraction:A Novel Sample Preparation Method for Chromatography[J].Journal of Chromatography A,1986,371(1):299-306.
[25]谢永荣,腾莉丽,余月容.微波法提取柑桔皮中天然色素[J].赣南师范学院学报,1994,(2):34-37.
[26]梅成.微波萃取技术的应用[J].中成药,2002,24(2):134-135.
[27]A.Zlotoraynski.The Application of Microwave Radiation to Aalytical and Environmental Chemistry[J].Critical Reviews in Analytical Chemistry,1995,(1):43.76.
[28]王艳,张铁军.微波萃取技术在中药有效成分提取中的应用[J].中草药,2005,36(3):470-473.
[29]M.E.Lucchesi,E Chemat,J.Smadja.Solvent-free Microwave Extraction of Essential Oil from Aromatic Herbs:Comparison with Conventional Hydro-distillation[J].Journal of Chromatography A,2004,1043(2):323-327.
[30]M.E.Lucchesi,F.Chemat,J.Smadja.An Original Solvent Free Microwave Extraction of Essential Oils from Spices[J].Flavour and Fragrance Journal,2004,19(2):134-138.
[31]张代佳,刘传斌,修志龙,昌增益.微波技术在植物胞内有效成分提取中的应用[J].中草药,2000,31(9):附5-6.
[32]J.R.J.Pare,M.Sigouin,J.Lapointe.Microwave-assisted Natural Products Extraction.1991,US Ptaent No.519588(5002784).
[33]J.R.J.Pare,J.M.R.Belnager,S.S.Stafford.Microwave-assisted Process (MAP~(TM)):A New Tool for the Analytical Laboratory[J].TrAC Trends in Analytical Chemistry,1994,13(4):176-184.
[34]D.R.Bgauhrst,D.M.P.Mingos.Design and Application of a Relfux Modification for the Synthesis of Organmetallic Compounds Using Microwave Dielectric Loss Hetaing Effects[J].Journal of Organometallic Chemistry,1990,384(3):C57-C60.
[35]D.R.Baghurst,S.R.Cooper,D.L.Greene,D.M.P.Mingos,S.M.Reynolds.Applictaion of Microwave Dielectric Loss Heating Effects for the Rapid and Convenient Synthesis of Coordination Compounds[J].Polyhedron,1990,9(6):893-895.
[36]冯年平,沈岚,韩朝阳,朱沪平,范广平.决明子微波萃取法与常用提取方法的比较[J].中成药,2004,26(3):189-191.
[37]李核,李攻科,张展霞.密闭系统中微波辅助萃取机制探讨[J].分析测试学报,2004,32(5):12-16.
[38]李核,李攻科,张展霞.影响微波辅助萃取虎杖中白黎芦醇产率的一些重要操作参数[J].分析化学,2003,31(11):1341-1344.
[39]李核,李攻科,张展霞.密闭式微波系统的微波辅助萃取动力学模型[J].中山大学学报(自然科学版),2004,43(3):40-44.
[40]符嫦娥,韩伟.微波萃取技术[J].化工技术与开发,2004,3(1):22-52.
[41]C.W.Huie.A Review of Modem Sample PerPartaion Techniques for the Extrctaion and Analysis of Medicine Plant[J].Bioanaltyical Chemisrty,2002,373(1-2):23-30.
[42]段胜林.微波辐射技术在食品萃取工业和化学工业上的应用[J].食品工业科技,1999,20(2):70-71.
[43]郝金玉,韩伟,邓修.新鲜银杏叶经微波辅助提取后微观结构的变化[J].中草药,2002,33(8):739-741.
[44]韩伟,高姗,邓修.微波辐射促进阔叶十大功劳叶萃取过程的研究[J].华东理工大学学报,2002,28(4):337-340.
[45]王娟,沈平攘,沈永嘉.微波辅助萃取葛根和刺五加微观机制的研究[J].中草药,2002,35(1):31-33.
[46]S.Chemat,H.Ant-Amar,A.Lagha,D.C.Esveld.Microwave-assisted Extraction Kinetics of Terpenes from Caraway Seeds[J].Chemical Engineering and Porcessing,2005,44(12):1320-1326.[47]沈岚,冯年平,韩朝阳.微波萃取对不同形态结构中药及含不同极性成分中药的选择性研究[J].中草药,2002,33(7):604-607. [48]王志祥,李红娟,万水昌,李菊,乐龙.微波萃取技术及其在中药有效成分提取中的应用[J].时珍国医国药,2007,18(5):1245-1247. [49]栾伟.石蒜中加兰他敏的微波辅助提取、分离和分析的研究[D].广州:中山大学,2004. [50]冯年平,范广平,吴春兰,韩朝阳.微波萃取技术在中药提取中的应用[J].世界科技技术-中药现代化
药物生产技术,2002,4(2):49-53. [51]刘川生,王平,王立飞,梅成,陈薇薇.微波萃取技术在天然药物提取中的研究进展[J].中国天然药物,2003,1(3):187-192. [52]郝金玉,韩伟,周永伟,刘海峰,邓修.微波萃取器内流体的沉降速度分布[J].化学工业与工程,2002,19(5):343-348. [53]Z.C.Kodba,J.Marsel.Microwave-assisted Extraction and Sonication of Polychlorobiphenils from River Sediments and Risk Assessment by Toxic Equivalency Factors[J].Chromatographia,1999,49(1-2):21-27. [54]J.C.Young.Microwave-assisted Extraction of the Fungal Metabolite Ergosterol and Total Fatty Acids[J].Journal of Agriculture and Food Chemistry,1995,43(11):2904-2910. [55][55]I.R.Pereiro,A.Wasik,R.Lobinski.Determination of Mercury Species in Fish Rreference Materials by Isothermal Multicapillary Gas Chromatography with Atomic Emission Detection after Microwave-assisted Solubilization and Solvent Extraction[J].Journal of Analytical Atomic Spectrometry,1998,13(8):743-747. [56]M.E.Lucchesi,F.Chemat,J.Smadja.An Original Solvent Free Microwave Extraction of Essential Oils from Spices[J].Flavour and Fragrance Journal,2004,19(2):134-138. [57]A.Pastor,E.Vázquez,R.Ciscar,M.de la Guardia.Efficiency of the Microwave-assisted Extraction of Hydrocarbons and Pesticides from Sediments [J].Analytica Chimica Acta,1997,344(3):241-249. [58]C.S.Eskilsson,E.Bj6rklund.Analytical-scale Microwave-assisted Extraction[J].Journal of Chromatography A,2000,902(1):227-250. [59]H.M.J.Pylypiw,T.L.Arsenault,C.M.Thetford,M.M.J.Incorvia.Suitability of Microwave-assisted Extraction for Multiresidue Pesticide Analysis of Produce [J].Journal of Agriculture and Food Chemistry,1997,45(9):3522-3528.
[60]M.P.Llompart,R.A.Lorenzo,R.Cela,K.Li,J.M.R.Belanger,J.R.J.Paré.Evaluation of SupercriticaI Fluid Extraction,Microwave-assisted Extraction and Sonication in the Determination of Some Phenolic Compounds from Various Soil Matrices[J].Journal of Chromatography A,1997,774(1-2):243-251.
[61]邓湘庆,龚盛昭.微波辅助萃取中药有效成分的研究进展[J].广东化工,2006,33(12):89-92.
[62]I.J.Barnabas,J.R.Dean,I.A.Fowlis,S.P.Owen.Extraction of Polycyclic Aromatic Hydrocarbons from Highly Contaminated Soils Using Microwave Energy[J].Analyst,1995,120:1897-1904.
[63]元英进,刘明言,董岸杰.中药现代化生产关键技术[M].北京:化学工业出版社,2002.
[64]C.Molins,E.A.Hogendoom,E.Dijkman,H.A.G.Heusinkveld,R.A.Baumann.Determination of Linuron and Related Compounds in Soil by Microwave-assisted Solvent Extraction and Reversed-phase Liquid Chromatography with UV Detection[J].Journal of Chromatography A,2000,869(1-2):487-496.
[65]M.Letellier,H.Budzinski.Influence of Sediment Grain Size on the Efficiency of Focused Microwave Extraction of Polycyclic Aromatic Hydrocarbons[J].Analyst,1999,124(1):5-14.
[66]J.A.Maria,M.R.B.Jacqueline,E C.Padilla,J.R.J.Paré.Influence of Solvent,Matrix Dielectric Properties,and Applied Power on the Liquid-phase Microwave-assisted Processes(MAP~(TM)) Extraction of Ginger[J].Food Research International,2003,36(5):499-504.
[67]孔臻,刘钟栋.微波法从苹果渣中提取果胶的研究[J].郑州粮食学报,2000,21(2):11-15.
[68]唐小俊,张名位,池建伟,张雁,施英,何焕清,张瑞芬.姬松茸多糖的微波辅助提取与含量测定[J].中国食品学报,2006,6(1):267-272.
[69]聂金媛,吴成岩,吴世容,李志良,微波辅助提取茯苓中茯苓多糖的研究[J].中草药,2004,35(12):1346-1348.
[70]黄璞,谢明勇,聂少平,陈奕,李昌,谢建华.响应曲面法优化微波辅助提取黑灵芝孢子多糖工艺研究[J].食品科学,2007,28(10):200-203.
[71]滑艳,邓雁如,汪汉卿.各种挥发油的药理活性及在医学方面的应用[J].天 然产物研究与开发,2003,15(5):467-470.
[72]Pare J R Jocelyn.1994,US5338557:Microwave Extraction of Volatile Oils.
[73]Pare J R Jocelyn.1995,US5458897:Microwave-assisted Extraction from Materials containing Organic Matter.
[74]Pare J R Jocelyn.1995,US5377426:Microwave-assisted Generation of Volatiles,of Supercritical Fluid,and Apparatus therefore.
[75]Pare J R Jocelyn.1996,US19947:Microwave-assisted Generation of Volatiles,of Supercritical Fluid,and Apparatus therefore.
[76]陈业高,海丽娜,毕先钧.微波辐射在天然药用活性成分提取分离中的应用[J].微波学报,2003,19(2):85-89.
[77]回瑞华,侯冬岩,李铁纯,关崇新.苦杏仁挥发油化学成分的微波-一时蒸馏萃取GC-MS分析[J].分析测试学报,2003,22(1):55-57.
[78]回瑞华,侯冬岩,李铁纯.微波-萃取木香挥发性化学成分的气相色谱-质谱分析[J].质谱学报,2003,24(4):471-476.
[79]回瑞华,侯冬岩,朱永强,刘晓媛.微波-同时蒸馏萃取分离肉桂挥发性成分分析[J].理化检验-化学分册,2006,42(2):105-108.
[80]赵金尧,陈春保,杨辉.赤芍及其相关药对中挥发油成分的研究[J].广州化学,2005,30(3):35-38.
[81]成玉怀,闰豫君,鲁建江.红景天叶中挥发油的微波提取初步实验[J].广东药学,2002,12(6):21-22.
[82]鲁建江,王莉,陈宏伟,孙萍.佩兰中挥发油的微波提取法[J].时珍国医国药,2001,12(9):774.
[83]谭仁祥.植物成分分析[M].北京:科学出版社.2000:386-413.
[84]高锦明.植物化学[M].北京:科学出版社,2003:217-254.
[85]M.Gao,W.Huang,M.RoyChowdhury,C.Z.Liu.Microwave-assisted Extraction of Scutellarin from Erigeron breviscapus Hand-Mazz and its Determination by High-performance Liquid Chromatography[J].Analytica Chimica Acta,2007,591(2):161-166.
[86]J.Y.Hao,W.Han,S.D.Huang,B.Y.Xue,X.Deng.Microwave-assisted Extraction of Artemisinin from Artemisia annua L[J].Separation and Purification Technology,2002,28(3):191-196.
[87]X.J.Pan,G.G.Niu,H.Z.Liu.Microwave-assisted Extraction of Tanshinones from Salvia miltiorrhiza bunge with Analysis by High-performance Liquid Chromatography[J].Journal of Chromatography A,2001,922(1-2):371-375.
[88]邹晓军,高小利.丹参中丹参素和原儿茶醛的微波提取工艺研究[J].中药材,2007,30(6):735-737.
[89]王楠.皂苷生物活性的研究进展[J].医学研究生学报,2007,20(2):211-214.
[90]刘永练,郑成,毛桃嫣,张新强,骆间仪.微波提取人参中活性成分人参皂苷的研究[J].广州大学学报(自然科学版),2006,5(6):52-55.
[91]Z.Y.Hu,M.Cai,H.H.Liang.Desirability Function Approach for the Optimization of Microwave-assisted Extraction of Saikosaponins from Radix Bupleuri[J].Separation and Purification Technology,2007,61:266-275.
[92]黎海彬.罗汉果皂苷的微波提取[J].食品科学,2007,28(3):143-147.
[93]程红霞,林强,程维明.苄基异喹啉类生物碱药理作用及机制的研究进展[J].中国新药与临床杂志,2006,25(5):392-397.
[94]刘覃,陈晓青,蒋新宇,吴升德.微波辅助提取龙葵中总生物碱的研究[J].天然产物研究与开发,2005,17(1):65-69.
[95]肖桂青,田云,卢向阳,方俊.微波辅助提取荷叶生物碱条件的优化[J].氨基酸和生物资源,2007,29(2):76-79.
[96]A.Brachet,P.Christten,J.I.Veuthcy.Focused Microwave-assisted Extraction of Cocaine and Benzoylecgonine from Coca Leaves[J].Phytochemical Analysis,2002,13(3):162-169.
[97]F.Zhang,B.Chen,S.Xiao,S.Z.Yao.Optimization and Comparison of Different Extraction Techniques for Sanguinarine and Chelerythrine in Fruits of Macleaya cordata(Willd) R.Br[J].Separation and Purification Technology,2005,42(3):283-290.
[98]江纪武.植物药有效成分手册[M].北京:人民卫生出版社,1986:3.
[99]李开泉,陈武,熊筱娟,王雪.乌索酸的化学、药理及临床应用进展[J].中成药,2002,24(9):709-711.
[100]L.Liu,W.R.Hudgins,S.Shack,M.Q.Yin,D.Samid.Cinnamic Acid:A Natural Product with Potential Use in Cancer Intervention[J].International Journal of Cancer,1995,62(3):345-350.
[101]王立新,韩广轩.齐墩果酸的化学及药理研究[J].药学实践杂志,2001,19(2):104-107.
[102]田瑛,董俊兴.天然产物中抗爱滋病病毒活性成分的研究进展[J].中国药学杂志,2002,37(6):401-406.
[103]郭锦棠,杨俊红,李雄勇,褚治德.微波与索氏提取甘草酸的正交买验研究[J].中国药学杂志,2002,37(12):919-922.
[104]孙秀利,秦培勇,谭天伟.微波法提取丹参中丹酚酸B的研究[J].中草药,2007,38(3):379-382.
[105]肖诗明,张忠,李勇,曾继光.苦荞麦麸皮中黄酮的提取工艺条件研究[J].食品科学,2006,27(1):156-158.
[106]张胜帮,赵玲玲.黄酮类化合物的提取纯化研究进展[J].温州大学学报·自然科学版,2007,28(5):25-29.
[107]陈斌,南庆贤,吕玲,周熙成.微波萃取葛根总异黄铜的工艺研究[J].农业工程学报,2001,17(6):123-126.
[108]Z.K.Guo,Q.H.Jin,G.Q.Fan,Y.P.Duan,C.Qin,M.J.Wen.Microwave-assisted Extraction of Effective Constituents from a Chinese Herbal Medicine Radix puerariae[J].Analytica Chimica Acta,2001,436(1):41-47.
[109]赵二劳,盖青青,张海容.微波萃取沙棘黄酮的研究[J].食品工业与发酵,2004,30(12):148-150
[110]朱蕾,王竹天,杨大进.葸醌类化合物的定性定量方法研究进展[J].中国食品卫生杂志,2006,18(2):155-158.
[111]吴拥军,孔娜,石杰,于斐,张洪权.中药巴戟天中蒽醌的提取与测定[J].安阳师范学院学报,2006(5):90-93.
[112]沈岚,冯年平,韩朝阳,朱沪平,范广平.大黄微波萃取法与常用提取方法的比较研究[J].中成药,2003,25(8):614-616.
[113]郝守祝,张虹,刘丽,李智恩,徐祖洪.微波技术在大黄游离蒽醌浸提中的应用[J].中草药,2002,33(1):23-26.
[114]张越华,曾和平.脂肪酸在生命过程中的作用研究进展[J].中国油脂,2006,31(12):11-16.
[115]马立红,王晓梅.多不饱和脂肪酸药理作用研究[J].吉林中医药,2006,26(12):69-70.
[116]李林强,李建科,刘迎利.超声波处理提取华山松籽油的研究[J].西北农林科技大学学报(自然科学版),2003,31(5):115-117.
[117]符嫦娥.微波萃取绿藻花生四烯酸及其纯化研究[M].华东理工大学硕士论文,20050120.
[118]范文洵.a-亚麻酸及其代谢产物EPA和DHA[J].生理科学进展,1988,19(2):110-113.
[119]邱磊.多不饱和脂肪酸的药理研究进展[J].药学实践杂志,1996,14(2):77-80.
[120]范亚苇,邓泽元,余永红,邓胜国,李静.不同脂肪酸甲酯化方法对共轭亚油酸分析的影响[J].中国油脂,2007,32(1):52-55.
[121]张亚刚,樊莉,文彬,马莉,吾满江·艾力.紫外可见分光光度法在共轭亚油酸定量分析中的应用[J].疆石油学院学报,2002,14(2):59-63.
[122]M.S.Manku.Analysis of γ-linolenic[J].Journal of Chromatographic Science,1983,8:1-11.
[123]Le-Ellen Dayhuff,Martha J.M.Wells.Identification of Fatty Acids in Fishes Collected from the Ohio River Using Gas Chromatography - Mass Spectrometry in Chemical Ionization and Electron Impact Modes[J].Journal of Chromatography A,2005,1098(1-2):144-149.
[124]徐秀兰,胡磊军,吴梧桐.脂肪酸的分析方法研究[J].药物生物技术,1998,5(3):161-165.
[125]郑立立,王磊,江克铮.鱼油中二十碳五烯酸和二十二碳六烯酸的气相色谱-红外光谱分析[J].分析化学,1994,2(4):383-385.
[126]赵先恩,索有瑞,王凌云,尤进茂.深海鱼油中脂肪酸的柱前衍生-高效液相色谱串联质谱分析[J].食品科学,2007,28(8):358-362.
[127]任其龙,熊任天,王宪达,吴平东.超临界流体色谱法分离二十碳五烯酸和二十二碳六烯酸[J].分析化学,2001,29(9):1076-1078.
[128]Tomá(?) Rezanka.Analysis of Polyunsaturated Fatty Acids Using High Performance Liquid Chromatography-Atmospheric Pressure Chemical Ionization Mass Spectrometry[J].Journal of High Resolution Chromatography,2000,23(4):338-342.
[129]T.K.Miwa,K.L.Mikolajczak,F.R.Earle,I.A.Wolff.Gas Chromatographic Characterization of Fatty Acids,Identification Constants for Mono- and Dicarboxylic Methyl Esters[J].Analticaly Chemistry,1960,32(13):1739-1742.
[130]徐学兵等.油脂化学[M].北京:中国商业出版社,1993:259-260.
[131]徐秀兰,胡磊军,吴梧桐.脂肪酸的分析方法研究[J].药物生物技术,1998,5(3):161-165.
[132]万新祥,张立.鱼油的药用价值[J].中国药学杂志,1990,25(7):392.
[133]C.D.Bannon,J.D.Craske,D.L.Felder,I.J.Garland,L.M.Norman.Analysis of Fatty Acid Methyl Esters with High Accuracy and Reliability:Ⅵ.Rapid Analysis by Split Injection Capillary Gas-Liquid Chromatography[J].Journal of Chromatography A,1987,407:231-241.
[134]D.E.Albertyn,C.D.Bannon,J.D.Craskeetal.Analysis of Fatty Acid Methyl Esters[J].Chromatographia,1982,247(3):71-74.
[135]K.Eder.Gas Chromatographic Analysis of Fatty Acid Methyl Esters[J].Journal of Chromatography B,1995,671(1-2):113-131.
[136]回瑞华,侯冬岩,李铁纯,李学成,刘晓媛,雷磊,国艳秋.食用植物油中脂肪酸的分析[J].鞍山师范学院学报,2006,8(6):19-21.
[137]邱磊,姜远英.多不饱和脂肪酸的药理研究进展[J].药学实志,1996,14(2):77-80.
[138]窦学廉,康毅.X-3多不饱和脂肪酸的药理研究进展[J].天津医科大学学报,1996,2(4):82-83.
[139]张金廷.脂肪酸及其深加工手册[M].北京:化工出版社,2002,8:362-363.
[140]张施军,朱薇,许颂.HP 4890D气相色谱仪在海豹油功效成分测定中的应用[J].水产科技情报,2000,27(2):169-171.
[141]曾惠玲.中药化学成分提取新技术研究进展[J].海峡药学,2005,17(5):1-3.
[142]王昌利,李君.中药有效成分提取方法研究进展[J].陕西中医函授,1995,(3):23-25.
[143]王昌利,范少敏.中药有效群体及有效成分提取分离方法研究进展[J].陕西中医学院学报,2001,24(6):60-62.
[144]李真,贾亮,贾绍义.中药有效成分提取技术及其应用[J].化学工业与工程,2005,22(6):450-455.
[145]李继遥,周学东,戴朝政,张萍.气相色谱及气相色谱-质谱联用技术分析牙菌斑脂肪酸方法的建立[J].华西口腔医学杂志,2000,18(6):386-388.
[146]李萍,刘丽芳.常用中药液相与气相色谱鉴定[M].北京:化学工业出版社,2005:19-20.
[147]张海松.中药猫爪草中挥发油和脂肪酸的气相色谱质谱联用分析[D].西安:陕西师范大学,2006。
[148]S.R.Heller,F.W.Melafferty,D.B.Stauffer,et al.GWA.EPA/NIH Mass Spectral Data Kase[M].Washington:US Government printing office,1978.
[149]丛浦珠.质谱学在天然有机化学中的应用[M].北京:科学出版社,1987.
[150]Y.Masada.Analysis of Essential Oils by Gas Chromatography and Mass Spectrometry[M].New York:John wile and sons.Inc.1976.
[151]张利,纪军,朱晓旺,吴圆圆,于环,张槟,李雪岭,孙喜琢.软脂酸诱导人肝癌HepG2细胞的凋亡[J].中国医学科学院学报,2004,26(6):671-676
[152]N.Fukuda,T.Etoh,K.Wada,et al.Differential Effects of Geometrical Isomers of Octadecadienoic Acids on Ketogenesis and Lipid Secretion in the Livers from Rats Fed a Cholesterol-enriched Diet[J].Annals of Nutrition and Metabolism,1995,39:185-192.
[153]李丕高,李西安,曹庆生.紫茉莉籽油的提取及其脂肪酸组成分析[J].中国油脂,2007,32(6):35-37
[154]余纲哲.鳗骨油的提取与分析[J].食品工业科技,1994,(3):66-69.
[155]汪茂田,谢培山,王忠东等编著.天然有机化合物提取分离与结构鉴定[M].化学工业出版社,2004:5.
[156]J.Bernard,Sciences et vie.2001,214:68.