中药的毛细管电泳指纹图谱的研究方法

目的介绍了毛细管电泳指纹图谱的优势，毛细管电泳指纹图谱的研究方法与评价方法及其在中药质量控制中的应用。方法以中药指纹图谱质量控制特征为基础，综述了毛细管电泳在中药指纹图谱方面应用的基础理论和方法。结果建立了一套完整的中药指纹图谱研究方法，包括实验条件的优化、系统适用性试验、电泳峰的指认与标定、双定性双定量相似度评价法等。结论数字化指纹图谱技术是数字中药质控的典型代表和核心技术，建立毛细管电泳数字化指纹图谱是实现中药现代质量控制的重要技术之一。     

用复杂性科学原理揭示中药指纹图谱的本质特征

目的对中药指纹图谱的本质特征进行深入研究。方法从复杂性科学角度论述中药指纹图谱所具有的本质特征。结果中药指纹图谱具有系统性、特征性、相对稳健性、模糊性、整体性、复杂性、动态开放性、活性交互性、微观精确性、宏观量化特征、超信息特征和数字化特征，总计12个本质特征。结论宏观定性评价是利用指纹图谱评价中药质量的基础和前提，宏观定量评价构成了中药指纹图谱控制中药质量的高级阶段。复杂性科学是指导中药指纹图谱控制中药质量的理论精髓。     

中药高效液相色谱指纹图谱在线专家系统设计与应用

目的设计中药色谱指纹图谱在线专家系统知识库和推理机。方法以中药材甘草为例，推荐其样品预处理方法、检测方法、分离模式和色谱优化条件。结果利用中药色谱指纹图谱在线专家系统推荐的实验方法建立了甘草HPLC指纹图谱，为科学评价与有效控制甘草质量提供了新途径。结论中药HPLC指纹图谱在线专家系统对甘草HPLC指纹图谱建立方法推荐真实有效，方案可行，效率高。     

清热解毒注射液指纹图谱多维多息特征的数字化评价

目的提出中药指纹图谱多维多息特征数字化评价方法，用F和I等37个指标揭示中药指纹图谱的多维多息特征。方法用自行研制的“中药指纹图谱多维多息特征数字化评价系统软件”评价清热解毒注射液的11味药材、中间体和制剂的HPLC指纹图谱实验结果，进行比较研究。结果从积分信号强度、信号均化程度、分离度、指纹信息量等多方面综合评价出金银花、黄芩、连翘、中间体和制剂的指纹图谱比较理想。结论F和I等37个指标可客观、真实、全面地揭示中药指纹图谱的多维多息的数字化特征。     

银翘解毒丸数字化指纹谱、对数谱、平方谱和反向指纹谱的多维评价方法研究

目的建立银翘解毒丸（Yinqiao Jiedu pill,YQJDP）高效液相色谱数字化指纹谱（N-FP）、对数指纹谱（ln-FP）、平方谱（S-FP）和反向谱（R-FP）。方法应用＂中药色谱指纹图谱超信息特征数字化评价系统4.0＂软件计算46个数字化参数进行潜信息特征数字化评价。用系统指纹定量法（systematically qualified fingerprint method,SQFM）评价YQJDPs在4种指纹谱图谱模式下的质量等级。结果在N-FP下15批YQJDPs的质量为：S3-S6及S8质量为1级;S2为3级;S7为2级,DS1-DS4及WS1-WS2质量为8级。结论本文所建立的多维指纹图谱评价方法可清晰地揭示YQJDPs超信息数字化特征,对数指纹谱能有效揭示中药指纹图谱各峰的均化性特征,消除批间差异增加指纹共性特征。平方谱和反向谱则能分别强调大峰和小峰在中药质量评价中的特异性作用。本文为中药指纹图谱合理评价中药质量提供一种参考方法。     

茶多酚静脉注射液高效液相指纹谱相关性研究

目的：对茶多酚注射液质量进行全面评价，将色谱数据提取为直观的图表。方法：采用HPLC指纹图谱技术，建立茶多酚静脉注射液指纹谱，并将多元统计方法应用于茶多酚静脉注射液的茶叶原料、注射液中间体以及注射液指纹谱。结果：主成分分析实现合理降维，聚类分析对样品准确分类，判别分析的正判率为100%，实现了指纹图谱的数字化。结论：本方法简便可靠，可以鉴别出不同制剂类型和不同处方工艺的样品。     

红外指纹图谱超信息特征数字化定量评价银杏叶片质量研究

目的建立银杏叶片(GT)红外指纹图谱和一阶导数光谱指纹图谱。以红外指纹图谱指数、信息量指数、波动量指数和信息波动量指数以及中红外指纹定量法理论,构建中红外指纹图谱超信息特征数字化定量评价方法,并评价GT质量。方法采用直接压片法,用傅立叶变换中红外光谱仪测定14批GT样品。结果依据GT红外指纹图谱超信息特征数字化、红外指纹定量法和一阶导数光谱指纹图谱定性、定量评价鉴定S4和S7为异常样品,S1、S2、S6和S12质量稍低,其余8批质量相对较好。结论本文利用数字化定量评价方法实现了中药红外图谱叠加信息的有效处理,并立足于整体定量角度建立红外系统指纹定量法,实现利用IRFP快速、简捷、准确地检验中药复杂系统总化学物含量,建立了中红外数字化定量指纹图谱评价中药质量的新方法。     

银黄注射液指纹图谱的建立及质量相关性研究

目的建立银黄注射液的指纹图谱。方法使用ZORBAXSB-C18色谱柱,流动相：乙睛-0.1%磷酸溶液进行梯度洗脱,检测波长为318nm,流速为1.00mL·min-1,柱温为25℃。结果利用2004年A版《中药色谱指纹图谱相似度评价系统》计算软件生成银黄注射液指纹图谱,确定12个共有峰,各峰分离度良好,符合指纹图谱检测要求。结论该方法简便、准确、重复性好,为评价银黄注射液质量提供依据。     

中药指纹图谱数据库的意义和现状

目的：探讨中药指纹图谱共享数据库的目的和意义。方法：检索国内文然资料并进行分析。结果：中药指纹图谱技术被认为是中药质量控制现代化的一种有效解决方案。中药指纹图谱技术的发展和完善是一个长期的过程，需要大量的资料和经验的积累，合理的保存和管理这些信息，必然对指纹图谱技术的发展产生巨大的推动作用。结论：中药指纹图谱数据库的研究已经滞后于中药指纹图谱技术的发展，应当加大中药指纹图谱共享数据库的研究力度。     

葛根与葛根提取物及葛根注射液指纹图谱研究

目的:建立葛根注射液的指纹图谱检测方法,研究葛根药材、葛根提取物和葛根注射液的共有成分的相关性.方法:用高效液相色谱法、二极管阵列检测器为检测方法,分析10批药材、提取物和注射液的共有峰.结果:用高效液相色谱法建立了葛根药材、葛根提取物和葛根注射液的指纹图谱,三者的相关性良好.结论:葛根药材、提取物及注射液相关性良好,各批样品图谱基本一致,因而工艺稳定,制剂的质量有保证.建立的指纹图谱检测方法可作为葛根提取物及其药材和注射液的质量评价的中药依据之一.     

Simultaneous determination of nine components in Qingkailing injection by HPLC/ELSD/DAD and its application to the quality control

High-performance liquid chromatography coupled with photo diode array detection and evaporative light scattering detection (HPLC/DAD/ELSD) was established to simultaneously determine nine ingredients in Qingkailing injection. Four wavelengths at 240, 254, 280 and 330 nm, respectively, were chosen as the monitoring wavelength to determine two nucleosides (uridine and adenosine), geniposide, baicalin and two organic acids (chlorogenic acid and caffeic acid), and an evaporative light scattering detector combined was employed to determine three steroids (cholic acid, ursodeoxycholic acid and hyodeoxycholic acid). This assay was fully validated in respect to precision, repeatability and accuracy. The proposed method was successfully applied to quantify the nine ingredients in 19 different Qingkailing injection samples and by principal component analysis (PCA) and hierarchical clustering analysis (HCA), it demonstrated significant variations in the content of these compounds in the samples from different manufacturers and preparation procedures. This method could be readily utilized as a quality control method for traditional Chinese medicine (TCM).     

高效液相色谱法测定清开灵注射液中绿原酸含量

目的建立检测清开灵注射液中绿原酸含量的高效液相色谱法。方法采用Shimadzu-C18色谱柱(150 mm×4.6 mm,5μm),流动相为乙腈-0.4%磷酸溶液(13∶87),检测波长327 nm,流速1.0 mL/min。结果绿原酸进样量在0.082 8～0.828 0μg范围内与峰面积线性关系良好,r=0.999 1(n=5);平均加样回收率为97.53%,RSD=1.21%(n=6)。结论所用方法准确可靠、重复性好,可用于清开灵注射液的质量控制。     

Quantitative analysis of betaine in Lycii Fructus by HILIC-ELSD

A rapid and simple high-performance liquid chromatography (HPLC) method with evaporative light scattering detection (ELSD) was developed for the determination of betaine from Lycii Fructus. Betaine was separated with an Atlantis hydrophilic interaction liquid chromatography silica column (4.6 × 150 mm, 5 μm, 100 Å) by isocratic elution using 30 mM ammonium acetate buffer and acetonitrile (20:80, v/v %) as the mobile phase. The flow rate was 1.0 mL/min, and the temperature for the spray chamber and drift tube was set at 30 and 50 °C, respectively. The method was fully validated with respect to linearity, precision, accuracy, stability and robustness. The HPLC/ELSD method was applied successfully to the quantification of betaine in the extract of Lycii Fructus. The HPLC analytical method for pattern recognition analysis was validated by repeated analysis of twenty-six L. barbarum L. from China (BC01–BC26), 3 L. barbarum L. (BJ27–BJ29) from Japan, 12 L. chinense Miller from China (CC30–CC41) and 51 L. chinense Miller samples (CK42–CK92) from Korea. The results indicate that the established HPLC/ELSD method is suitable for quality evaluation of Lycii Fructus.     

HPLC指纹图谱结合系统聚类分析法对灵芝孢子油质量的研究

目的:建立灵芝孢子油的高效液相色谱指纹图谱,并结合聚类分析法初步考察不同采收时间、产地及破壁工艺对灵芝孢子油质量的影响。方法:采用反相高效液相色谱法测定灵芝孢子油中甘油三油酸酯的含量,色谱柱为LiChrospher RP-18e(250mm×4.6mm,5μm),流动相为甲醇-异丙醇(梯度洗脱),蒸发光散射检测器检测。采用系统聚类法对灵芝孢子油样品色谱中各特征峰的相对峰面积进行分析。结果:系统聚类法将供试品分成两大类,其中采收时间及破壁工艺对灵芝孢子油的质量影响明显,产地影响则不明显。结论:该方法能较好地为灵芝孢子油的质量评估提供有益的信息。     

中药复方制剂中黄芩苷含量的HPLC检测法的建立

目的建立中药复方制剂中黄芩苷含量的HPLC检测法。方法采用高效液相色谱法检测以清开灵颗粒为代表的中药复方制剂中黄芩苷的含量,流动相为0.5%磷酸水溶液-甲醇(58︰42),检测波长280nm,流速为1.0mL/min,采用外标峰面积法计算清开灵颗粒中黄芩苷的含量。结果黄芩苷与有关物质完全分离,在0.1019～1.019μg范围内峰面积与浓度呈现良好的线性关系(R2=0.9999,n=5),平均回收率为99.44%(RSD=0.86%,n=5)。结论本实验方法简单、迅速、专一性强,适用于中药复方制剂中黄芩苷的含量检测。     

Quality evaluation of Polygala japonica through simultaneous determination of six bioactive triterpenoid saponins by HPLC-ELSD

Polygala japonica Houtt (Polygalaceae), a traditional Chinese herb, has been used as expectorant, anti-inflammatory, antibacterial and antidepressant agent. To evaluate the quality of P. japonica, a high performance liquid chromatography (HPLC) with evaporative light scattering detector (ELSD) method was developed for the simultaneous determination of six active triterpenoid saponins. With a Discovery C(18) analytical column, the analytes were separated efficiently using acetonitrile-methanol-0.05% trifluoroacetic acid (TFA) as mobile phase in a gradient program. The evaporator tube temperature of ELSD was set at 105 degrees C, and with the nebulizing gas flow-rate of 2.6l/min. All calibration curves showed good linear regression (gamma>0.9991) within the tested range. Additionally, reproducibility for the quantification of six saponins in P. japonica with intra- and inter-day variations of less than 5.0% was observed. Quantification of the six active saponins in P. japonica from different locations was performed by this newly developed method, which provides a new tool for the assessment of quality of P. japonica.     

清开灵软胶囊中胆酸和猪去氧胆酸的含量测定

目的建立清开灵软胶囊中胆酸和猪去氧胆酸的高效液相色谱-蒸发光散射(HPLC-ELSD)含量测定方法。方法采用ShiseidoCapcell MGⅡC18色谱柱(150 mm×4.6 mm,5μm),以甲醇-乙腈-0.5%冰醋酸溶液(49∶20∶31)为流动相,流速为1.0 mL/min,柱温为25℃,蒸发光散射检测器,漂移管温度为108℃,载气流速为2.8 L/min。结果胆酸和猪去氧胆酸的进样量分别在2.338～18.704μg(r=0.999 4)和2.018～16.141μg(r=0.999 5)范围内与各自的峰面积积分值呈良好的对数线性关系,平均回收率分别为98.51%和98.01%,RSD分别为0.74%和0.72%(n=9)。结论所用方法简便、准确、分离效果好,适用于该制剂的质量控制。     

Simultaneous determination of Saikosaponin a,c and d in different parts of wild bupleurum from Shanxi Province

Asa traditional Chinese herbal medicine exhibiting analgesic, fever-reducing and anti-inflammatory effects, Radix Bupleuri (Chai-Hu) is commonly used for the treatment of influenza, which is derived from the dried roots of Bupleurum chinense DC. and Bupleurum scorzonerifolium Willd. Among of diverse chemical components, saikosaponins are the key active components of the herb medicine. In the present study, we established a method of high performance liquid chromatography (HPLC) coupled with evaporative light scattering detection (ELSD) for simultaneous determination of saikosaponin a, c and d in root, stem, leaf and flower of Bupleurumchinense (B chinense) collected from different areas of Shanxi Province, China. The results from 16 samples of root, stem, leaf and flower of B chinense demonstrated that the total contents of the three saikosaponins in the root of B chinense collected from Dongshan Taiyuan, Xishan, Tianlongshan and Pangquangou were 4.26 mg/g, 3.22 mg/g, 4.23 mg/g and 3.05 mg/g, respectively. However, there was scarcely any saikosaponins in the stem, leaf and flower of B chinensecollected from above-mentioned areas. The method of HPLC coupled with ELSD was suitable for quality control of Radix Bupleuri. The result also confirmed that the root of B chinense was the best medicinal part.     

HPLC法测定清开灵口服液中绿原酸的含量

目的：建立用HPLC法测定清开灵口服液中绿原酸的含量．方法：采用日本岛津SHIMADZU LC-2010A型液相色谱仪,ULTIMATE AQ—C18色谱柱,检测波长327nm,以甲醇-0．2mol／L磷酸二氢钠（调pH至3．2）（15：85）为流动相,流速为0．8ml／min。结果：精密度及回收率结果良好,平均回收率为99．67％（n=10）,RSD=1．30％。结论：方法准确可靠,可用于清开灵口服液中绿原酸的含量测定．     

A validated method for quantitative determination of saponins in notoginseng (Panax notoginseng) using high‐performance liquid chromatography with evaporative light‐scattering detection

A gradient high‐performance liquid chromatographic (HPLC) method with evaporative light‐scattering detection (ELSD) for the determination of major saponins in a Chinese traditional herbal medicine, Panax notoginseng, is described. Samples were analysed by means of a reverse‐phase column (Waters Spherisorb ODS‐2, C‐18) using acetonitrile and water under gradient conditions as the mobile phase over 60 min. The ELSD used was set at an evaporating temperature of 35°C and pressurized air pressure of 3.4 bars. The detection limit (signal/noise > 3) of the saponins was 50 ng. The method was validated by inter‐ and intra‐day assays and recovery tests.