过程分析技术在丹参注射液醇沉和养胃颗粒喷雾制粒中的应用研究
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摘要
我国的中药生产工艺落后,缺乏有效的在线监测技术,难以保证中药产品的质量。近红外光谱分析技术作为一种快速、无损的过程分析方法,已在众多领域得到应用。近年来,近红外光谱技术在中药制造过程的应用研究也逐渐增多,然而,其在中药喷雾制粒和醇沉过程分析中的应用研究鲜有报道。本文以养胃颗粒喷雾制粒和丹参注射液醇沉过程为具体研究对象,开展了近红外光谱分析技术在中药喷雾制粒和醇沉过程中的应用研究,主要内容包括:
1.建立了同时测定无糖型养胃颗粒中没食子酸、芍药内酯苷、芍药苷和苯甲酰芍药苷含量的HPLC分析方法。该法分离效果好,方法简便、准确,适用于无糖型养胃颗粒的质量控制。
2.将近红外光谱分析技术和移动块标准偏差法相结合,建立了一种可快速判断养胃颗粒喷雾制粒干燥终点的过程分析方法;同时建立了近红外光谱分析方法快速测定养胃颗粒中水分含量的方法。
3.采用正交试验设计法,选择浓缩液密度、搅拌速度、乙醇加入速度、乙醇浓度、静置时间、冷藏温度和冷藏时间为考察因素,综合考虑各试验条件下醇沉液中丹参素含量、原儿茶醛含量和含固量,方差分析结果表明,乙醇浓度和丹参浓缩液密度对考察指标有较大影响。
4.以正交试验结果为基础,以近红外光谱法为分析手段,建立了一种快速判别丹参注射液醇沉工艺稳定性的方法。以丹参注射液醇沉过程为例,采集各个醇沉条件下的近红外光谱图,建立近红外光谱的主成分分析模型,对生产工艺参数的变化进行判别。
5.以偏最小二乘法(PLS)为建模方法,建立了可同时快速测定丹参注射液醇沉过程中丹参素、原儿茶醛和含固量的近红外定量分析方法。
Traditional Chinese Medicine (TCM) is a historic industry in China, and its manufacture has been highly depended on experience. An effective on-line monitoring technique is absolutely necessary for the quality control of TCM. As a fast, non-destructive process analysis method, Near-Infrared Spectroscopy (NIRS) technique has been applied in many fields of industry, but a little in TCM manufacturing process. In this thesis, the application of NIRS technique to on-line quality analysis of TCM manufacturing process including Salvia miltiorrhiza ethanol precipitation and 'YangWei' Granules spraying and drying granulation had been researched. The main content was summarized as follows:
1. An HPLC method was established for determining gallic acid, albiflorin, paeoniflorin, and benzoylpaenoniflorin in Sugar-free 'YangWei' Granules. The developed HPLC method provided an accurate and sensitive way to quantitative analysis of gallic acid, albiflorin, paeoniflorin and benzoylpaenoniflorin in Sugar-free 'YangWei' Granules. It was suitable for the reference for NIR.
2. On the basis of the result of HPLC analysis, taken spray granulation process of 'YanWei' Granules as an example to develop a rapid method to monitor the endpoint in the process of flidized-bed spray granulation. Measure the content of water in products by the NIR model, and use Moving Block of Standard Deviation (MBSD) to judge the endpoint of the process.
3. If the parameter was changed, the precipitation result would be changed subsequently. Taking ethanol precipitation process of Salvia miltiorrhiza as an example, the orthogonal experimental design was utilized to choose the most important ones from the following factors: the original cream concentration (ρ), first precipitation stirring velocity (V), first precipitation affiliate rate(x), first ethanol concentration (C), first static time (T), first cold temperature (W) and first frozen time (t). Evaluating with tanshinol content, protocatechuic aldehyde content, solid content and combined score, we found out thatρand C were the most influential factors. In order to verify the results, another experiment was carried out, whose results were consistent.
4. On the basis of the results of orthogonal experiments, a NIR method was established to fast distinguish the stability of technics. Taking ethanol precipitation process of Salvia miltiorrhiza as an example, various spectrograms under different conditions were collected. Compared principal component analysis (PCA) models with different pretreatment methods and bands, finally chose the MSC pretreatment and 7070-9500 cm'1 band to establish PCA models. Analysed the spectrograms with PCA method under different ethanol content, batches of cream, cold temperature, sizes containers and numbers of precipitation. And it was found out that the different precipitation conditions could be distinguished using above PCA method.
5. An online content analysis method was established to monitor Salvia miltiorrhiza ethanol precipitation process. A partial least squares (PLS) model was established using the selected wave bands, to measure the content of tanshinol, protocatechuic aldehyde and solid matters. It was proved that the model was competent for online analysis of Salvia miltiorrhiza ethanol precipitation process.
1.建立了同时测定无糖型养胃颗粒中没食子酸、芍药内酯苷、芍药苷和苯甲酰芍药苷含量的HPLC分析方法。该法分离效果好,方法简便、准确,适用于无糖型养胃颗粒的质量控制。
2.将近红外光谱分析技术和移动块标准偏差法相结合,建立了一种可快速判断养胃颗粒喷雾制粒干燥终点的过程分析方法;同时建立了近红外光谱分析方法快速测定养胃颗粒中水分含量的方法。
3.采用正交试验设计法,选择浓缩液密度、搅拌速度、乙醇加入速度、乙醇浓度、静置时间、冷藏温度和冷藏时间为考察因素,综合考虑各试验条件下醇沉液中丹参素含量、原儿茶醛含量和含固量,方差分析结果表明,乙醇浓度和丹参浓缩液密度对考察指标有较大影响。
4.以正交试验结果为基础,以近红外光谱法为分析手段,建立了一种快速判别丹参注射液醇沉工艺稳定性的方法。以丹参注射液醇沉过程为例,采集各个醇沉条件下的近红外光谱图,建立近红外光谱的主成分分析模型,对生产工艺参数的变化进行判别。
5.以偏最小二乘法(PLS)为建模方法,建立了可同时快速测定丹参注射液醇沉过程中丹参素、原儿茶醛和含固量的近红外定量分析方法。
Traditional Chinese Medicine (TCM) is a historic industry in China, and its manufacture has been highly depended on experience. An effective on-line monitoring technique is absolutely necessary for the quality control of TCM. As a fast, non-destructive process analysis method, Near-Infrared Spectroscopy (NIRS) technique has been applied in many fields of industry, but a little in TCM manufacturing process. In this thesis, the application of NIRS technique to on-line quality analysis of TCM manufacturing process including Salvia miltiorrhiza ethanol precipitation and 'YangWei' Granules spraying and drying granulation had been researched. The main content was summarized as follows:
1. An HPLC method was established for determining gallic acid, albiflorin, paeoniflorin, and benzoylpaenoniflorin in Sugar-free 'YangWei' Granules. The developed HPLC method provided an accurate and sensitive way to quantitative analysis of gallic acid, albiflorin, paeoniflorin and benzoylpaenoniflorin in Sugar-free 'YangWei' Granules. It was suitable for the reference for NIR.
2. On the basis of the result of HPLC analysis, taken spray granulation process of 'YanWei' Granules as an example to develop a rapid method to monitor the endpoint in the process of flidized-bed spray granulation. Measure the content of water in products by the NIR model, and use Moving Block of Standard Deviation (MBSD) to judge the endpoint of the process.
3. If the parameter was changed, the precipitation result would be changed subsequently. Taking ethanol precipitation process of Salvia miltiorrhiza as an example, the orthogonal experimental design was utilized to choose the most important ones from the following factors: the original cream concentration (ρ), first precipitation stirring velocity (V), first precipitation affiliate rate(x), first ethanol concentration (C), first static time (T), first cold temperature (W) and first frozen time (t). Evaluating with tanshinol content, protocatechuic aldehyde content, solid content and combined score, we found out thatρand C were the most influential factors. In order to verify the results, another experiment was carried out, whose results were consistent.
4. On the basis of the results of orthogonal experiments, a NIR method was established to fast distinguish the stability of technics. Taking ethanol precipitation process of Salvia miltiorrhiza as an example, various spectrograms under different conditions were collected. Compared principal component analysis (PCA) models with different pretreatment methods and bands, finally chose the MSC pretreatment and 7070-9500 cm'1 band to establish PCA models. Analysed the spectrograms with PCA method under different ethanol content, batches of cream, cold temperature, sizes containers and numbers of precipitation. And it was found out that the different precipitation conditions could be distinguished using above PCA method.
5. An online content analysis method was established to monitor Salvia miltiorrhiza ethanol precipitation process. A partial least squares (PLS) model was established using the selected wave bands, to measure the content of tanshinol, protocatechuic aldehyde and solid matters. It was proved that the model was competent for online analysis of Salvia miltiorrhiza ethanol precipitation process.
引文
[1]肖培根,肖小河.21世纪与中药现代化.中国中药杂志,2000,25(2):67-70
[2]http://www.fda.gov/Cder/OPS/PAT.htm
[3]刘全.近红外过程分析技术在制药行业质量控制中的应用.当代中国近红外光谱技 术,2006,1:773-777
[4]Blanco M,Villarroya I..Trends in Analytical Chemistry.2002,21(4):240-250
[5]吴立军.天然药物化学.人民卫生出版社,2003,6:19
[6]胡冠时.中草药除鞣质方法的研究.中草药.1991,22(11):491
[7]孙月霞,吴淑娥.浓缩液密度对醇沉效果的影响.基层中药杂志,2000,5(14):36
[8]邵锡宸.中草药醇沉工艺与设备浅析.医药工程设计,1995,4:23-26
[9]王彦波,杨淑英.水提醇沉工艺中用醇量的经验公式.中成药,1999,21(11):609-610
[10]杨建春,杜国辉,于桂兰.益母草口服液醇沉工艺的改进.中国医院药学杂志,2003,6(23):359
[11]林德祥,邱巨香,陈叶明.正交试验法优选云芝多糖醇沉工艺的研究.南京中医药大学学报,2005,5(21):328-330
[12]马刚欣.清热解毒口服液醇沉工艺的优选.中成药,2006,28(3):439-440
[13]周本杰,郭谦.小儿健脾消食口服液醇沉工艺研究.中药材,2003,10(26):757-758
[14]韩桂茹,陈太平.水提醇沉对中药各类有效成分的影响.中国中药杂志,1993,18(5):286
[15]杨海燕,陈福明,阎武.醇沉对纯化金银花中绿原酸工艺的影响.中成药,2006,28(9):1256-1259
[16]张华.醇沉浓度对补气生血口服液所含成分的影响.中成药,2006,28(8):1204-1207
[17]刘晓华,卢琴.活血胶囊制备工艺研究.中成药,1997,19(8):6
[18]伍沅.干燥技术的进展和应用.化学工程,1995,23(3):47-56
[19]端木志宏,林光伟.流化床喷雾制粒技术在中药生产中的应用.中成药,1992,14(9):9-10
[20]Ennis B J..A microlevel-based characterization of granulation phenomena.Powder Technology.1991,65:257-272
[21]李昭华.中药喷雾干燥生产经验介绍.中成药,2003,25(3):256-257
[22]王秀良,向大雄,赵绪元.不同赋形剂及配方对中药喷雾干燥浓缩液粉制粒的影响.中成药,2002,24(2):90-92
[23]潘强,王世岭,贾立华,郭晓华,吴坤.喷雾干燥制备康复欣胶囊颗粒的影响因素.中国药业,2004,3(13):52-53
[24]林军.清淋颗粒喷雾干燥制粒工艺研究.中国中药杂志.2003,1(28):88-89
[25]张志兰.流化床喷雾制粒在枫蓼肠胃康无糖颗粒制备中的应用.中国医院药学杂志,2006,8(26):1043-1044
[26]吴拥军,李伟,相秉仁.光纤近红外漫反射光谱技术在前胡族植物分类中的应用探讨.计算机与应用化学,2000,17(2):111-112
[27]吴拥军,李伟,相秉仁.近红外光谱技术用于白芷类中药的鉴定研究.中药材,2001,24(1):26-8
[28]刘沭华,张学工,周群,孙素琴.模式识别和红外光谱法相结合鉴别中药材产地.光谱学与光谱分析,2005,6(25):878-881
[29]Woo Y.A.,Kim H.J.,JungHwan C..Discrimination of herbal medicines according to geographical origin with near infrared reflectance spectroscopy and pattern recognition techniques.Journal of Pharmaceutical and Biomedical Analysis,1999,21:407-413
[30]Woo YA,Cho C H,Kim H J,et al.Classification of cultivation area of ginseng by near infrared spectroscopy and ICP2AES.Microchem.J,2002,73(3):299-306
[31]邢旺兴,刘荔荔.不同产地红曲的近红外漫反射光谱聚类分析鉴别.中药材,2001,24(8):561-563
[32]Kudo M.,Watt RA.,Moffat A.C..Rapid identification of digitalis purpurea using near-infrared reflectance spectroscopy.Journal of Pharmacy & Pharmacology,2000,52(10):1271-1277
[33]Laasonen M.,Harmia-Puikkinen T.,Simard C.L..Fast identification of Echinacea purpurea dried roots using near-infrared spectroscopy.Analytical Chemistry,2002,74(11):2493-2499
[34]黄宝康,朱斌,郑汉臣.不同产地楮实子及伪品的近红外漫反射指纹图谱聚类分析.中药材,12(25):874-875
[35]杨海雷,瞿海斌,程翼宇.近红外漫反射光谱法快速无损鉴别阿胶真伪.光谱学与光谱分析,2006,26(1):60-62
[36]杨南林,瞿海斌,程翼宇.近红外光谱法快速测定三七总皂苷的方法研究.浙江大学学报(工学版),2002,36(4):463-466
[37]Guixing R.,Feng C..Simultaneous Quantification of Ginsenosides in American Ginseng(panax quinquefolium)Root Power by Visible/Near-Infrared Reflectance Spectroscopy.J Agric Food Chem,1999,47:2771-2775
[38]严诗楷,罗国安,王义明,程翼宇.栀子药材提取工艺的近红外光谱实时控制方法研究.光谱学与光谱分析,2006,26(6):1026-1030
[39]龚益飞,刘雪松,章顺楠,瞿海斌,程翼宇.近红外光谱法在线判断滴丸料液混合终点.中国药学杂志,2007,42(7)
[40]柯博克,刘雪松,陈勇,李文,瞿海斌,程翼宇.近红外光谱快速测定复方丹参滴丸的包衣厚度.中草药,2006,37(5):685-688
[41]Berntsson O.,Zackrisson G.,Ostling G..Determination of moisture in hard gelatin capsules using near-infrared spectroscopy:applications to at-line process control of pharmaceutics,Journal Of Pharmaceutical and Biomedical Analysis(England),1997,15(7):895-900
[42]Blanco M.,Coello J.,Iturriaga H.,Maspoch S.,et al.Determination of water in ferrous lactate by near infrared reflectance spectroscopy with a fiber optic probe,Journal of Pharmaceutical and Biomedical Analysis(England),1997,16(2):255-262
[43]Steck E.,Tarczynski F.,Walker D.S..Comparison of near-infrared methods for pharmaceutical product drying:In situ vs.effluent sampling,Appl Spectrosc,2001,55(8):1109-1111
[44]Plugge W.,Van Der Vlies C..Near-infrared spectroscopy as an alternative to assess compliance of ampicillin trihydrate with compendial specifications,Journal of Pharmaceutical and Biomedical Analysis(England),1993,11(6):435-442
[45]Last I.R.,Prebble K.A..Suitability of near infrared methods for the determination of moisture in a freeze-dried injection product containing different amounts of the active ingredient,Journal of Pharmaceutical and Biomedical Analysis(England),1993,11(11-12):1071-1076
[46]Kamat M.S.,Lodder R.A.,DeLuca P.P..Near-infrared spectroscopic determination of residual moisture in lyophilized sucrose through intact glass vials,Pharmaceutical Research(USA),1989,6:961-965
[47]Jones J.A.,Last I.R.,MacDonald B.F.,Prebble K.A..Development and transferability of near infrared methods for determination of moisture in a freeze-dried injection product,Journal of Pharmaceutical and Biomedical Analysis(England),1993,11(11-12):1227-1231
[48]Carpenter J.F.,Prestrelski S.J.,Dong A..Application of infrared spectroscopy to development of stable lyophilized protein formulations,European Journal of Pharmaceutics & Biopharmaceutics,1998,45(3):231-238
[49]Henkel L.,Hennig H..In-process measurement of moisture content in fluid beds,part 2.operational infrared moisture measurement,Pharmazeutische Industrie(Germany),1992,54(12):1047-1049
[50]White J.G..On-line moisture detection for a microwave vacuum dryer,Pharmaceutical Research,1994,11:728-732
[51]Frake P.,Greenhalgh D.,Grierson S.M..Process control and end point determination of a fluid bed granulation by application of near infrared spectroscopy,International Journal of Pharmaceutics-(Netherlands),1997,151:75-80
[52]Goebel S.G.,Steffens K.J..Online measurement of moisture and particle size in the fluidized-bed processing with the near-infrared-spectroscopy,Pharmazeutische Industrie(Germany),1998,60(10):889-895
[53]Rantanen J.,Yliruusi J..Determination of particle size in a fluidized bed granulator with a near infrared setup,Pharmacy and Pharmacology Communications(England),1998,4:73-75
[54]Rantanen J.,Lehtola S.,Ramet P.,et al.On-line monitoring of moisture content in an instrumented fluidized bed granulator with a multi-channel NIR moisture sensor,Powder Technol,1998,99(2):163-170
[55]Faure A.,York P.,Rowe R.C..Process control and scale-up of pharmaceutical wet granulation processes:a review,Eur J Pharm Biopharm,2001,52(3):269-277
[56]杨南林,程翼宇,瞿海斌.一种用于中药纯化过程的近红外光谱分析新方法.化学学报,2003,6 1(5):742-747
[57]瞿海斌,叶颖雅,程翼宇.近红外光谱快速鉴别丹参基地药材.药物分析杂志,2006,26(10)
[58]虞科,胡楚楚,程翼宇.近红外光谱法测定复方丹参滴丸中的3种有效成分.中国药学杂志,2006,41(3):226-229
[59]刘全,瞿海斌,程翼宇.用于渗漉提取过程分析的中药有效组分近红外光谱快速测定法.化工学报,200.3,54(11):1586-1591
[60]瞿海斌,李斌,刘雪松,程翼宇.红参醇提液浓缩过程近红外光谱在线分析方法。中国药学杂志,2005,40(24):1897-1899
[61]叶正良,虞科,程翼宇.一种基于小波变换的近红外化学指纹图谱分析方法.高等学校化学学报,2007,28(3):441-444
[62]虞科,程翼宇.一种基于最小二乘支持向量机算法的近红外光谱判别分析方法.分析化学,2006,34(4):561-564
[1]季宇彬.中药有效成分药理与应用.黑龙江科学技术出版社,1995:203
[2]李俊,梁君山.白芍总甙对B淋巴细胞增殖和白介素生成的调节作用.中国药理学与毒理学杂志,1994,8(1):53
[3]梁君山,陈敏珠.白芍总甙对大鼠腹腔巨噬细胞功能的影响.中国药理学与毒理学杂志,1990,4(2):153-154
[4]梁君山,陈敏珠.白芍总甙对大鼠佐剂性关节及其免疫功能的影响.中国药理学与毒理学杂志,1990,4(4):258
[5]Sonja Sekulic S.,Wakeman J.,Doherty P.,et al.Automated system for the on-line monitoring of powder blending processes using near-infrared spectroscopy Part Ⅱ.Qualitative approaches to blend evaluation[J].J.Pharm.Biomed.Anal.1998,17(8):1285-1309
[6]Blanco M.,Gozalez Bano R.,Bertran E..Monitoring powder blending in pharmaceutical processes by use of near infrared spectroscopy[J].Talanta.2002,56(1):203-212
[7]Chen YX,Sorensen LK..Determination of marker constituents in radix Glycyrrhizae and radix Notoginseng by near infrared spectroscopy,Fresenius Journal of Analytical Chemistry,2000,367(5):491-496
[1]张文生,李德坤,叶正良.反相高效液相色谱法测定丹参提取物中丹参素、原儿茶醛和丹酚酸B的含量.药物分析杂志,2003,23(6):475-476
[2]孙月霞,吴淑娥.浓缩液密度对醇沉效果的影响.基层中药杂志,2000,5(14):36
[3]周本杰,郭谦.小儿健脾消食口服液醇沉工艺研究.中药材,2003,10(26):757-758
[4]姚玉英.化工流体流动与传热.天津大学出版社.1999,8:193
[5]张风雷,李立纪,吴荣祖,刘培儒.正交法用于附子水提醇沉工艺研究.中成药,2005,27(7):833-834
[6]夏泉.正交设计优化黄精多糖的水提醇沉工艺.中国药师,2006,10(9):905-906
[1]虞科,胡楚楚,程翼宇.近红外光谱法测定复方丹参滴丸中的3种有效成分.中国药学杂志,2006,41(3):226-229
[2]Savitzky A,Golay M..Smoothing and differentiation of data by simplified least squares procedures.Analytical Chemistry,1964,36(8):1627-1639
[3]Gorry PA.General least-squares smoothing and differentitation by the convolution(Savitzky-Golay)Method.Analytical Chemistry,1990,62(6):570-573
[4] Karstang TV, Kvalheim O.. Multivariate prediction and background correction using local modeling and derivative spectroscopy. Analytical Chemistry, 1991,63(8): 767-772
[5] Osten DW, Kowalski BR... Background detection and correction in multicomponent analysis. Analytical Chemistry, 1985, 57(4): 908-917
[6] Tahboub YR, Pardue HL.. Evaluation of multiwavelength first- and second-derivative spectra for the quantitation of mixtures of polynuclear aromatic hydrocarbons. Analytical Chemistry, 1985, 57(1): 38-41
[7] Spiegelman CH, Mcshane MJ, Goetz MJ, et al. Theoretical justification of wavelength election in PLS calibration: development of a new algorithm. Analytical Chemistry, 1998, 70(1): 35-44
[2]http://www.fda.gov/Cder/OPS/PAT.htm
[3]刘全.近红外过程分析技术在制药行业质量控制中的应用.当代中国近红外光谱技 术,2006,1:773-777
[4]Blanco M,Villarroya I..Trends in Analytical Chemistry.2002,21(4):240-250
[5]吴立军.天然药物化学.人民卫生出版社,2003,6:19
[6]胡冠时.中草药除鞣质方法的研究.中草药.1991,22(11):491
[7]孙月霞,吴淑娥.浓缩液密度对醇沉效果的影响.基层中药杂志,2000,5(14):36
[8]邵锡宸.中草药醇沉工艺与设备浅析.医药工程设计,1995,4:23-26
[9]王彦波,杨淑英.水提醇沉工艺中用醇量的经验公式.中成药,1999,21(11):609-610
[10]杨建春,杜国辉,于桂兰.益母草口服液醇沉工艺的改进.中国医院药学杂志,2003,6(23):359
[11]林德祥,邱巨香,陈叶明.正交试验法优选云芝多糖醇沉工艺的研究.南京中医药大学学报,2005,5(21):328-330
[12]马刚欣.清热解毒口服液醇沉工艺的优选.中成药,2006,28(3):439-440
[13]周本杰,郭谦.小儿健脾消食口服液醇沉工艺研究.中药材,2003,10(26):757-758
[14]韩桂茹,陈太平.水提醇沉对中药各类有效成分的影响.中国中药杂志,1993,18(5):286
[15]杨海燕,陈福明,阎武.醇沉对纯化金银花中绿原酸工艺的影响.中成药,2006,28(9):1256-1259
[16]张华.醇沉浓度对补气生血口服液所含成分的影响.中成药,2006,28(8):1204-1207
[17]刘晓华,卢琴.活血胶囊制备工艺研究.中成药,1997,19(8):6
[18]伍沅.干燥技术的进展和应用.化学工程,1995,23(3):47-56
[19]端木志宏,林光伟.流化床喷雾制粒技术在中药生产中的应用.中成药,1992,14(9):9-10
[20]Ennis B J..A microlevel-based characterization of granulation phenomena.Powder Technology.1991,65:257-272
[21]李昭华.中药喷雾干燥生产经验介绍.中成药,2003,25(3):256-257
[22]王秀良,向大雄,赵绪元.不同赋形剂及配方对中药喷雾干燥浓缩液粉制粒的影响.中成药,2002,24(2):90-92
[23]潘强,王世岭,贾立华,郭晓华,吴坤.喷雾干燥制备康复欣胶囊颗粒的影响因素.中国药业,2004,3(13):52-53
[24]林军.清淋颗粒喷雾干燥制粒工艺研究.中国中药杂志.2003,1(28):88-89
[25]张志兰.流化床喷雾制粒在枫蓼肠胃康无糖颗粒制备中的应用.中国医院药学杂志,2006,8(26):1043-1044
[26]吴拥军,李伟,相秉仁.光纤近红外漫反射光谱技术在前胡族植物分类中的应用探讨.计算机与应用化学,2000,17(2):111-112
[27]吴拥军,李伟,相秉仁.近红外光谱技术用于白芷类中药的鉴定研究.中药材,2001,24(1):26-8
[28]刘沭华,张学工,周群,孙素琴.模式识别和红外光谱法相结合鉴别中药材产地.光谱学与光谱分析,2005,6(25):878-881
[29]Woo Y.A.,Kim H.J.,JungHwan C..Discrimination of herbal medicines according to geographical origin with near infrared reflectance spectroscopy and pattern recognition techniques.Journal of Pharmaceutical and Biomedical Analysis,1999,21:407-413
[30]Woo YA,Cho C H,Kim H J,et al.Classification of cultivation area of ginseng by near infrared spectroscopy and ICP2AES.Microchem.J,2002,73(3):299-306
[31]邢旺兴,刘荔荔.不同产地红曲的近红外漫反射光谱聚类分析鉴别.中药材,2001,24(8):561-563
[32]Kudo M.,Watt RA.,Moffat A.C..Rapid identification of digitalis purpurea using near-infrared reflectance spectroscopy.Journal of Pharmacy & Pharmacology,2000,52(10):1271-1277
[33]Laasonen M.,Harmia-Puikkinen T.,Simard C.L..Fast identification of Echinacea purpurea dried roots using near-infrared spectroscopy.Analytical Chemistry,2002,74(11):2493-2499
[34]黄宝康,朱斌,郑汉臣.不同产地楮实子及伪品的近红外漫反射指纹图谱聚类分析.中药材,12(25):874-875
[35]杨海雷,瞿海斌,程翼宇.近红外漫反射光谱法快速无损鉴别阿胶真伪.光谱学与光谱分析,2006,26(1):60-62
[36]杨南林,瞿海斌,程翼宇.近红外光谱法快速测定三七总皂苷的方法研究.浙江大学学报(工学版),2002,36(4):463-466
[37]Guixing R.,Feng C..Simultaneous Quantification of Ginsenosides in American Ginseng(panax quinquefolium)Root Power by Visible/Near-Infrared Reflectance Spectroscopy.J Agric Food Chem,1999,47:2771-2775
[38]严诗楷,罗国安,王义明,程翼宇.栀子药材提取工艺的近红外光谱实时控制方法研究.光谱学与光谱分析,2006,26(6):1026-1030
[39]龚益飞,刘雪松,章顺楠,瞿海斌,程翼宇.近红外光谱法在线判断滴丸料液混合终点.中国药学杂志,2007,42(7)
[40]柯博克,刘雪松,陈勇,李文,瞿海斌,程翼宇.近红外光谱快速测定复方丹参滴丸的包衣厚度.中草药,2006,37(5):685-688
[41]Berntsson O.,Zackrisson G.,Ostling G..Determination of moisture in hard gelatin capsules using near-infrared spectroscopy:applications to at-line process control of pharmaceutics,Journal Of Pharmaceutical and Biomedical Analysis(England),1997,15(7):895-900
[42]Blanco M.,Coello J.,Iturriaga H.,Maspoch S.,et al.Determination of water in ferrous lactate by near infrared reflectance spectroscopy with a fiber optic probe,Journal of Pharmaceutical and Biomedical Analysis(England),1997,16(2):255-262
[43]Steck E.,Tarczynski F.,Walker D.S..Comparison of near-infrared methods for pharmaceutical product drying:In situ vs.effluent sampling,Appl Spectrosc,2001,55(8):1109-1111
[44]Plugge W.,Van Der Vlies C..Near-infrared spectroscopy as an alternative to assess compliance of ampicillin trihydrate with compendial specifications,Journal of Pharmaceutical and Biomedical Analysis(England),1993,11(6):435-442
[45]Last I.R.,Prebble K.A..Suitability of near infrared methods for the determination of moisture in a freeze-dried injection product containing different amounts of the active ingredient,Journal of Pharmaceutical and Biomedical Analysis(England),1993,11(11-12):1071-1076
[46]Kamat M.S.,Lodder R.A.,DeLuca P.P..Near-infrared spectroscopic determination of residual moisture in lyophilized sucrose through intact glass vials,Pharmaceutical Research(USA),1989,6:961-965
[47]Jones J.A.,Last I.R.,MacDonald B.F.,Prebble K.A..Development and transferability of near infrared methods for determination of moisture in a freeze-dried injection product,Journal of Pharmaceutical and Biomedical Analysis(England),1993,11(11-12):1227-1231
[48]Carpenter J.F.,Prestrelski S.J.,Dong A..Application of infrared spectroscopy to development of stable lyophilized protein formulations,European Journal of Pharmaceutics & Biopharmaceutics,1998,45(3):231-238
[49]Henkel L.,Hennig H..In-process measurement of moisture content in fluid beds,part 2.operational infrared moisture measurement,Pharmazeutische Industrie(Germany),1992,54(12):1047-1049
[50]White J.G..On-line moisture detection for a microwave vacuum dryer,Pharmaceutical Research,1994,11:728-732
[51]Frake P.,Greenhalgh D.,Grierson S.M..Process control and end point determination of a fluid bed granulation by application of near infrared spectroscopy,International Journal of Pharmaceutics-(Netherlands),1997,151:75-80
[52]Goebel S.G.,Steffens K.J..Online measurement of moisture and particle size in the fluidized-bed processing with the near-infrared-spectroscopy,Pharmazeutische Industrie(Germany),1998,60(10):889-895
[53]Rantanen J.,Yliruusi J..Determination of particle size in a fluidized bed granulator with a near infrared setup,Pharmacy and Pharmacology Communications(England),1998,4:73-75
[54]Rantanen J.,Lehtola S.,Ramet P.,et al.On-line monitoring of moisture content in an instrumented fluidized bed granulator with a multi-channel NIR moisture sensor,Powder Technol,1998,99(2):163-170
[55]Faure A.,York P.,Rowe R.C..Process control and scale-up of pharmaceutical wet granulation processes:a review,Eur J Pharm Biopharm,2001,52(3):269-277
[56]杨南林,程翼宇,瞿海斌.一种用于中药纯化过程的近红外光谱分析新方法.化学学报,2003,6 1(5):742-747
[57]瞿海斌,叶颖雅,程翼宇.近红外光谱快速鉴别丹参基地药材.药物分析杂志,2006,26(10)
[58]虞科,胡楚楚,程翼宇.近红外光谱法测定复方丹参滴丸中的3种有效成分.中国药学杂志,2006,41(3):226-229
[59]刘全,瞿海斌,程翼宇.用于渗漉提取过程分析的中药有效组分近红外光谱快速测定法.化工学报,200.3,54(11):1586-1591
[60]瞿海斌,李斌,刘雪松,程翼宇.红参醇提液浓缩过程近红外光谱在线分析方法。中国药学杂志,2005,40(24):1897-1899
[61]叶正良,虞科,程翼宇.一种基于小波变换的近红外化学指纹图谱分析方法.高等学校化学学报,2007,28(3):441-444
[62]虞科,程翼宇.一种基于最小二乘支持向量机算法的近红外光谱判别分析方法.分析化学,2006,34(4):561-564
[1]季宇彬.中药有效成分药理与应用.黑龙江科学技术出版社,1995:203
[2]李俊,梁君山.白芍总甙对B淋巴细胞增殖和白介素生成的调节作用.中国药理学与毒理学杂志,1994,8(1):53
[3]梁君山,陈敏珠.白芍总甙对大鼠腹腔巨噬细胞功能的影响.中国药理学与毒理学杂志,1990,4(2):153-154
[4]梁君山,陈敏珠.白芍总甙对大鼠佐剂性关节及其免疫功能的影响.中国药理学与毒理学杂志,1990,4(4):258
[5]Sonja Sekulic S.,Wakeman J.,Doherty P.,et al.Automated system for the on-line monitoring of powder blending processes using near-infrared spectroscopy Part Ⅱ.Qualitative approaches to blend evaluation[J].J.Pharm.Biomed.Anal.1998,17(8):1285-1309
[6]Blanco M.,Gozalez Bano R.,Bertran E..Monitoring powder blending in pharmaceutical processes by use of near infrared spectroscopy[J].Talanta.2002,56(1):203-212
[7]Chen YX,Sorensen LK..Determination of marker constituents in radix Glycyrrhizae and radix Notoginseng by near infrared spectroscopy,Fresenius Journal of Analytical Chemistry,2000,367(5):491-496
[1]张文生,李德坤,叶正良.反相高效液相色谱法测定丹参提取物中丹参素、原儿茶醛和丹酚酸B的含量.药物分析杂志,2003,23(6):475-476
[2]孙月霞,吴淑娥.浓缩液密度对醇沉效果的影响.基层中药杂志,2000,5(14):36
[3]周本杰,郭谦.小儿健脾消食口服液醇沉工艺研究.中药材,2003,10(26):757-758
[4]姚玉英.化工流体流动与传热.天津大学出版社.1999,8:193
[5]张风雷,李立纪,吴荣祖,刘培儒.正交法用于附子水提醇沉工艺研究.中成药,2005,27(7):833-834
[6]夏泉.正交设计优化黄精多糖的水提醇沉工艺.中国药师,2006,10(9):905-906
[1]虞科,胡楚楚,程翼宇.近红外光谱法测定复方丹参滴丸中的3种有效成分.中国药学杂志,2006,41(3):226-229
[2]Savitzky A,Golay M..Smoothing and differentiation of data by simplified least squares procedures.Analytical Chemistry,1964,36(8):1627-1639
[3]Gorry PA.General least-squares smoothing and differentitation by the convolution(Savitzky-Golay)Method.Analytical Chemistry,1990,62(6):570-573
[4] Karstang TV, Kvalheim O.. Multivariate prediction and background correction using local modeling and derivative spectroscopy. Analytical Chemistry, 1991,63(8): 767-772
[5] Osten DW, Kowalski BR... Background detection and correction in multicomponent analysis. Analytical Chemistry, 1985, 57(4): 908-917
[6] Tahboub YR, Pardue HL.. Evaluation of multiwavelength first- and second-derivative spectra for the quantitation of mixtures of polynuclear aromatic hydrocarbons. Analytical Chemistry, 1985, 57(1): 38-41
[7] Spiegelman CH, Mcshane MJ, Goetz MJ, et al. Theoretical justification of wavelength election in PLS calibration: development of a new algorithm. Analytical Chemistry, 1998, 70(1): 35-44
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