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??OBJECTIVE To explore the active ingredients of wine fried Ligustrum lucidum fructus by studying the relationship between the HPLC chromatogram and antioxidant activity. METHODS The characteristic chromatogram of wine fried Ligustrum lucidum fructus processed by means of classical homothermal acceleration was established by HPLC. DPPH, ABTS, and FRAP METHODS were established to determine the antioxidant activity. The spectrum-effect relationship was studied by using partial least squares regression (PLSR), and the chromatographic peaks related to antioxidant activity were identified. RESULTS Peaks 1, 3, 8, 10, 14 and 15 were found to have positive relationship with DPPH free radical and ABTS free radical scavenging activity among the 17 matching characteristic chromatograms. Peaks 3, 8, 12, and 13 were significantly positively related to Fe³⁺ resuction capacity. Among the chromatographic peaks, peak 3 and peak 8 were positively related to the activities of scavenging DPPH free radical and ABTS free radical and reducing Fe³⁺. Peaks 3, 12, 13, 14, 15, and 17 were determined as salidroside, luteolin-7-O-glucoside, specnuezhenide, oleuropein, ligustroflavone, and luteolin, respectively. CONCLUSION The pharmcodynamic effects of wine fried Ligustrum lucidum fructus do not depend on the contents of several index components such as specnuezhenide and salidroside. The quality of traditional Chinese medicines should be represented by the compound groups associated with pharmcodynamic effect.     

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??OBJECTIVE To establish the HPLC fingerprint of Rhodiola crenulata herbs from Sichuan plateau, and compare them with commercially available samples. METHODS RP-HPLC analysis was applied using Agilent Zorbax C₁₈ chromatographic column (4.6 mm??250 mm,5 ??m). The mobile phase A was 0.1% formic acid aqueous solution and mobile phase B was 0.1% formic acid in acetonitrile. The flow rate was 1 mL??min^-1 and the column temperature was maintained at 35 ??. The detection wavelength was set at 245 nm and injection of sample was 20 ??L. The traditional Chinese medicine fingerprint chromatogram similarity evaluation system (Version 2004A), principal component analysis, and cluster analysis were used to compare 30 Rhodiola crenulata samples from various locations based on their HPLC chromatograms. RESULTS The established HPLC fingerprint of Rhodiola crenulata was able to analyze Rhodiola crenulata from different sources. CONCLUSION The method has good repeatability and stability, and can be used for the quality management standard of Rhodiola crenulata.     

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??OBJECTIVE To establish the fingerprint of Aconitum Flarum Hand. Mazz Busch. METHODS UPLC analysis was performed on ACQUITY UPLC BEH C₁₈ column(2.1 mm??50 mm,1.7 ??m). Gradient elution was conducted. Mobile A was 0.2% formic acid and 0.005% TFA in water; mobile B was methanol; and mobile C was acetonitrile. The flow rate was 0.3 mL??min^-1. The detection was carried out at 275 nm. The column temperature was maitained at 35 ??. The injection volume was 1.0 ??L. RESULTS The UPLC fingerprint of Aconitum Flarum Hand. Mazz was established, and 14 common peaks were found including the peaks of two major constituents. The similarity factors ranged from 0.850 to 0.980. In addition, there was significant difference between wild and cultivated samples. CONCLUSION This UPLC method has satisfactory precision, stability, repeatability and specificity. It provides a scientific method for identifying wild and cultivated Aconitum Flarum Hand. Mazz using fingerprint.     

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??OBJECTIVE To establish the quality evaluation method of the aerial roots of Ficus microcarpa L.f. based on their anti-inflammation activity. METHODS Twenty batches of samples from different producing areas were analyzed by HPLC on a Shimadzu Capcell Pak C₁₈ column(4.6 mm??250 mm,5 ??m)gradiently eluted with mobile phase of methanol and 0.1% formic acid aqueous at a flow rate of 1.0 mL??min^-1. The detection wavelength was set at 254 nm, and the column temperature was maintained at 35 ??. The chromatograms were analyzed by the software ??Similarity Evaluation System for Chromatographic Fingerprint of TCMs (Version 2012.1)?? and the common peaks were obtained. The anti-inflammatory effects of the aerial roots of Ficus microcarpa L.f. were assessed by murine model of xylene-induced ear edema. Spectrum-effect relationship was analyzed by bivariate correlation analysis using SPSS21.0. RESULTS Seventeen common peaks were identified in the HPLC fingerprints of 20 batches of aerial roots of Ficus microcarpa L.f. The anti-inflammatory effect of samples from Guangdong was better than those from Guangxi and Fujian (P<0.01). According to the result of spectrum-effect relationship analysis, six common peaks were closely related to the anti-inflammatory effects of the aerial roots of Ficus microcarpa L.f. (P<0.05). Cluster analysis was then carried out based on the six common peaks in order to divide the samples into different groups. CONCLUSION The quality evaluation method established in this research is successfully employed in the quality evaluation of the aerial root of Ficus microcarpa L.f..     

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??OBJECTIVE To establish the HPLC fingerprints of Amomum villosum Lour., Amomum villosum Lour. var. xanthioides T. L. Wu et Senjen and Amomum longiligulare T. L. Wu and find their differences. METHODS The samples were extracted with 75% ethanol aqueous and then analysis was carried out on an Agilent ZORBAX SB-Aq C₁₈ column with the mobile phase consisting of methanol (A) and 0.05% formic acid solution (B). Gradient elution (0 min, 5% A; 5 min, 5% A??15% A; 10 min, 15% A??26% A; 20 min, 26% A??40% A; 45 min, 40% A??70% A; 58 min, 70% A??100% A, 63 min, 100% A) was carried out at the flow rate of 1.0 mL??min^-1. The column temperature was maintained at 30 ??, and the detection wavelength was set at 263 nm. The software ??Similarity Evaluation System for Chromatographic Fingerprint of TCMs (Version 2012.0) ?? was employed to generate the mean chromatogras and carry out the similarity analysis of the samples. SPSS21.0 was employed to carry out the cluster analysis. RESULTS The HPLC fingerprints of the three varieties were different according to fingerprinting and cluster analysis. Amomum villosum Lour. var. xanthioides T. L. Wu et Senjen was obvilously differernt from Amomum villosum Lour. and Amomum longiligulare T. L. Wu. There were 25 common peaks in the former HPLC fingerprint and 29 common peaks in the latter. CONCLUSION The HPLC fingerprints of three kinds of Amomum villasums were set up for the first time and they provide reference for the identification and quality control of Amomum villosum Lour., Amomum villosum Lour. var. xanthioides T. L. Wu et Senjen, and Amomum longiligulare T. L. Wu.     

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??OBJECTIVE To study the content determination method of crotamiton. METHODS The quantitative mass balance method, HPLC external standard method and nuclear magnetic resonance(QNMR) were used to determine the content of crotamiton, respectively. The accuracy of the three methods was evaluated. RESULTS The contents of crotamiton were 99.2%,102.9% and 99.1% respectively as determined by the three different methods. CONCLUSION Because the ultraviolet absorption coefficients of cis- and trans-crotamiton might be different, the current pharmacopoeia method, ie, using integrated peak areas to calculate the content, is questionable. QNMR method can measure the contents of cis- and trans-crotamiton respectively, so it can be a complementary method to establish the reference standard.     

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??OBJECTIVE To establish a new dissolution method of Ligustrazine Phosphate Pills, which provides reference for revising the quality standard. METHODS The dissolution media were hydrochloric acid solution(pH 1.2), acetate buffer solution(pH 4.5), phosphate buffer solution(pH 6.8) and water. The dissolution curves of six batches of Ligustrazine Phosphate Pills in the four kinds of dissolution media were compared to establish the dissolution method. Apparatus 2 was used for the new method of dissolution test,using 500 mL water as the dissolution medium,at the rate of 75 r??min^-1. The dissolution solution was taken at 20 min and analyzed by HPLC. The dissolution limit was set at 80%. RESULTS The dissolution curves of the six batches of samples were similar in the four kinds of dissolution media. The pills were dissolved completely within 15 min. CONCLUSION The determination method is highly reproducible, accurate and reliable, which can objectively reflect the dissolution of ligustrazine phosphate pills, and provides a basis for the reasonable unification and revision of the dissolution test of the current quality standard.     

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??OBJECTIVE To explore the accumulation rules of the effective constituents in Ophiopogonis Radix to provide theoretical support for its production and quality control. METHODS Ophiopogonis Radix samples in different growth phases were harvested, and the total polysaccharides, total flavones, and total saponins in the sampleswere measured by ultraviolet spectrophotometry. Methylophiopogonanone A, ophiopogonin C, ophiopogonin D, and ophiopogonin D?? were determined by HPLC. RESULTS The contents of total polysaccharides, total flavones, and total saponins in Ophiopogonis Radix were positively correlated with root growth time. The contents of three categories of constituents increased with the prolongation of root growth time, but the accumulative rate was inconsistent in different growth phases, which had a slight decrease after reaching the maximum at the end of March. The accumulation trend of six single components were basically the same to the three categories of constituents. For samples with same harvest time, the content of the main constituents was higher in the samples treated by paclobutrazol than those without paclobutrazol treatment. CONCLUSION The variation trend of the main chemical components in Ophiopogonis Radix is basically the same to that of the root growth. Methylophiopogonanone A and phiopogonin D are the most representative, and they could be taken as evaluation index to guide production and quality control of Ophiopogonis Radix.     

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??OBJECTIVE To establish an HPLC method for rapid screening and simultaneous determination of 10 preservatives in eye drops and assess their antimicrobial effectiveness. METHODS A Waters XBridge C₁₈ column (4.6 mm??150 mm,5 ??m) was used, and the mobile phase was 0.1% phosphoric acid-methanol-THF eluted in gradient mode at a flow rate of 1.0 mL??min^-1. The detection wavelength was set at 214 nm. The antimicrobial effectiveness of the preservatives was assessed according to Ch. P 2015. RESULTS The calibration curves were linear in the range of the corresponding test concentrations (r=0.999 3-1.000 0). The recoveries were between 96.1%-101.8%. One of the eye drops products did not meet the requirement of Ch. P 2015. CONCLUSION The established method is rapid and inexpensive. And it ensures excellent simplicity, sensitivity, specificity, and reproducibility and can be used for rapid screening and determination of the contents of preservatives in eye drops. The amount of preservatives should be established during the R&D period or determined according to the RESULTS of antimicrobial effectiveness test rather than using empirical values.     

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??OBJECTIVE To establish an HPLC-TQ-MS/MS assay for simultaneous determination of berberine, plantamajoside, saikosaponin a, tetrahydropalmatine, paeoniflorin and amygdalin in rat plasma and investigate the pharmacokinetics of Jiawei Baiteng extracts in rats. METHODS The separation was achieved on an Agilent Poroshell 120 EC-C₁₈ column(3.0 mm??100 mm,2.7 ??m) at 35 ??. The mobile phase was consisted of 0.05% formic acid aqueous solution and acetonitrile containing 0.05% formic acid, eluting with a gradient procedure. Mass spectrometry was performed in the multiple reaction monitoring (MRM) mode, with programmed ionization modes witching and time segment scanning. The ion reactions for quantification were as follows: m/z 335.9??m/z 319.9(berberine, ESI⁺), m/z 639.1??m/z 160.9(plantamajoside, ESI^-),m/z 779.3??m/z 617.4(saikosaponin a, ESI^-),m/z 356.0??m/z 192.0(tetrahydropalmatine,ESI⁺),m/z 449.1??m/z 121.1(paeoniflorin, ESI^-),m/z 456.1??m/z 323.1(amygdalin, ESI^-),m/z 323.9??m/z 126.9(gliclazide, internal standard, ESI⁺) and m/z 321.9??m/z 170.1 (gliclazide, internal standard, ESI^-). Blood samples were collected in heparinized tubes via the retinal venous plexus from each rat after a single oral dose of Jiawei Baiteng extracts(3.1 g??kg^-1). The plasma samples were pretreated by methanol precipitation to remove protein components, and then analyzed by HPLC-TQ-MS/MS. The pharmacokinetic parameters of the bioactive components of Jiawei Baitengex tracts in rats were calculated by DAS (Drug and Statistics for Windows) software(Version 2.0). RESULTS The methodological test showed that the linear concentration ranges of berberine, plantamajoside, saikosaponin a, tetrahydropalmatine, paeoniflorin and amygdalin were 0.59-292.50, 0.68-168.75, 6.05-1 512.50, 0.68-337.50, 6.70-1 675.00 and 5.60-1 400.00 ng??mL^-1, respectively. The limits of quantification (LOQs) of the six analytes were 0.59,0.68,6.05,0.68,6.70 and 5.60 ng??mL^-1, respectively. The HPLC-TQ-MS/MS method was also validated with good precision, recovery and stability, which conformed to the analytical standards of biological samples. CONCLUSION The established method is proved to be sensitive, simple and reliable, which is suitable for the pharmacokinetic study of Jiawei Baiteng extracts.     

不同产地栀子的UPLC指纹图谱

目的:建立不同产地栀子的UPLC指纹图谱,为其质量控制提供比较全面快速的评价方法。方法:实验对26批不同产地的栀子和1批水栀子样品进行UPLC指纹图谱的检测,采用ACQUITY UPLCHSS T3色谱柱(2.1 mm×100 mm,1.8μm),乙腈-0.05%磷酸溶液为流动相梯度洗脱,流速0.4 m L·min-1,检测波长265 nm,采用相似度分析,聚类分析和主成分分析方法对27批样品的指纹图谱进行分析。结果:建立了26批栀子样品的共有图谱,确定了23个共有峰,对8个峰进行了指认,26批栀子与对照图谱相似度0.96,栀子对照图谱与水栀子相似度为0.935,聚类分析在已有样本间也可以将水栀子与栀子分开,主成分分析结果江西产栀子水平较高,质量较一致。结论:该实验建立的栀子UPLC指纹图谱可以为栀子的质量控制提供科学的评价。     

UPLC指纹图谱结合化学模式识别评价不同产地五灵脂药材质量

目的:建立五灵脂药材的超高效液相色谱法(UPLC)指纹图谱,结合化学模式识别法评价不同产地五灵脂药材质量。方法:采用UPLC建立指纹图谱,色谱柱为ACQUITY UPLC HSS T3(150 mm×2.1 mm,1.8μm),流动相为乙腈-0.1%磷酸水溶液(梯度洗脱),检测波长为265 nm,流速为0.25 mL·min^-1,柱温为30℃,进样量为1.0μL。结合相似度评价、聚类热图分析及正交偏最小二乘法-判别分析(OPLS-DA)综合评价不同产地五灵脂药材质量。结果:建立的五灵脂药材UPLC指纹图谱共标定14个共有峰,指认出其中6个成分,分别为原儿茶酸、4-羟基苯甲酸、苯甲酸、槲皮苷、穗花杉双黄酮、扁柏双黄酮;22批五灵脂药材相似度为0.870~0.998;聚类热图分析将22批五灵脂药材分为两类,陕西省商洛市所产五灵脂可与其他产区样品完全区分;OPLS-DA共筛选出7个质量差异标志性成分。结论:建立的五灵脂药材UPLC指纹图谱及其化学模式识别方法稳定可行,可为五灵脂药材质量研究提供参考。     

栀子质量的化学模式识别研究

目的采用高效液相色谱法及聚类法建立栀子药材质量评价的化学模式识别方法。方法采用反相高效液相法,可变波长紫外检测器,Eclipse XDB-C18色谱柱,乙腈-0.1%磷酸水溶液梯度洗脱,检测波长238 nm(0～20 min,检测环烯醚萜苷类成分)、440 nm(20～30 min,检测西红花苷类成分),以24批栀子共有色谱峰峰面积为基础进行聚类分析。结果主成分分析和系统聚类分析结果基本一致,24批栀子样品可分为3类。结论此方法可较系统地用于栀子的质量控制。     

沉香化气丸的UPLC指纹图谱与化学模式识别

目的:建立沉香化气丸的超高效液相色谱(UPLC)指纹图谱,为评价该制剂的整体质量提供参考依据。方法:采用Phenomenex Kinetex C_(18)色谱柱(4.6 mm×100 mm,2.7μm),流动相乙腈(A)-0.1%磷酸水溶液(B)梯度洗脱(0~7 min,12%~16%A;7~14 min,16%~19%A;14~16 min,19%~25%A;16~19 min,25%~28%A;19~22 min,28%~42%A;22~27 min,42%~46%A;27~33 min,46%~48%A;33~37 min,48%~72%A;37~39 min,72%~90%A;39~42 min,90%A),分段变波长测定(0~3 min,285 nm;3~20 min,210 nm;20~24 min,254 nm;24~42 min,210 nm),进样量2μL,流速调整至0.8 mL·min~(-1);根据相似度评价,结合化学计量学方法对沉香化气丸进行质量评价。结果:建立了20批沉香化气丸的UPLC指纹图谱,标定了27个共有峰,通过对照品指认了12个共有峰,20批样品指纹图谱的相似度均0.98。通过聚类分析可将样品聚为3类,结合主成分分析、正交偏最小二乘法-判别分析发现7个成分是造成不同批次样品差异性的主要标记物。结论:指纹图谱的构建与化学模式识别可为沉香化气丸的质量控制提供更为全面的信息参考。建立的UPLC指纹图谱方法稳定可行。     

江西不同产区车前子药材的HPLC指纹图谱及其多成分化学模式识别分析

目的:建立车前子HPLC指纹图谱检测方法,结合化学模式识别方法对江西不同产区车前子样品进行分析,并测定其中5种有效成分的含量,为科学评价和有效控制该药材的质量提供参考。方法:利用HPLC检测34批车前子药材,采用"中药色谱指纹图谱相似度评价系统"(2012版)进行相似度评价,以其色谱峰信息为数据来源,利用化学模式识别方法综合分析江西道地药材车前子的质量,对筛选并指认出的5个有效成分京尼平苷酸、大车前苷、毛蕊花糖苷、木犀草苷、异毛蕊花糖苷进行定量分析。结果:江西不同产区车前子样品的相似度均 0. 86,说明江西不同产区车前子相似度良好。利用正交偏最小二乘法-判别分析能较好地区分不同产区车前子药材,且可判断与车前子质量相关性较强的化学成分。5种有效成分的含量在不同产区车前子中仍存在一定差异,其中尤以大车前苷的含量差别较大。结论:建立的车前子HPLC指纹图谱特征性强,结合化学模式识别方法可有效的评价车前子质量并区分其不同产区,可为该药材的质量控制提供参考依据。     

吴茱萸指纹图谱及化学模式识别研究

目的： 采用HPLC梯度洗脱法研究34批吴茱萸药材样品的色谱图,对不同产地、不同品种的吴茱萸中药材采用指纹图谱相似度评价及聚类分析和主成分分析等化学模式识别技术进行研究,以期为吴茱萸中药材品种鉴别与品质评控提供参考。方法： 色谱条件为Ultimate XB-C₁₈色谱柱（4.6 mm×150.0 mm,3 μm）,流动相乙腈-1%乙酸水溶液梯度洗脱,流速0.8 mL·min^-1,检测波长245 nm,进样量10 μL,柱温25℃。结果： 34批样品有11个共有峰,共有峰保留时间的RSD<1%,峰面积的RSD比较大。各批次药材品质较为一致,化学成分组成及含量上均存在一定差异。聚类分析及主成分分析从化学成分上揭示了2010年版《中国药典》规定3种吴茱萸中药材种质的远近关系。结论： 以指纹图谱数据为基础,将聚类分析与主成分分析结合起来不仅可以进行吴茱萸中药材的质量控制乃至品种鉴别,还可以为下一步制定新的吴茱萸质量控制模式提供参考依据。     

不同产地佛手指纹图谱及模式识别研究

目的：建立不同产地佛手指纹图谱,利用模式识别方法比较不同产地佛手的差异。方法：本文采用高效液相色谱法对4个产地25批佛手建立高效液相指纹图谱,利用相似度评价技术、聚类分析、主成分分析进行分析研究。结果：从已建立的佛手指纹图谱中确定26个共有峰,指认出4个共有峰,利用聚类分析、主成分分析可区分佛手产地。结论：研究结果表明,不同地理位置佛手药材相似度存在一定差异,地理位置相近的佛手药材相似度较高。     

栀子叶化学成分

目的:研究栀子叶的化学成分,为该资源的深度开发和利用提供初步的科学依据。方法:采用硅胶柱色谱、凝胶柱色谱、大孔吸附树脂及ODS柱色谱等分离手段,对采自南京溧水县的栀子叶95%乙醇提取物乙酸乙酯部位及水相浸膏进行分离纯化,利用1H-NMR,13C-NMR等多种波谱学数据及理化性质确定其化学结构。结果:从栀子叶中分离得到8个化合物,经结构鉴定为β-gardiol(1),α-gardiol(2),β-谷甾醇(3),山柰酚(4),槲皮素(5),京尼平苷(6),栀子苷(7),β-胡萝卜苷(8)。结论:化合物1,2,4~7为首次从栀子叶中分离得到。     

不同产地金银花药材的UPLC指纹图谱分析

目的： 建立不同产地金银花药材的超高效液相特征性指纹图谱,为有效控制和科学评价金银花药材整体质量提供依据。 方法： 采用Agilent C₁₈ 色谱柱（2.1 mm×50 mm,1.8 μm）,流动相乙腈-0.2%磷酸水,以0.4 mL·min^-1的流速进行梯度洗脱,检测波长238 nm,柱温30 ℃。 结果： 在21 min内得到金银花药材的指纹图谱,对其中5个色谱峰进行了初步归属,并对14批药材样品进行了分析,其相似度为0.915~0.987。 结论： UPLC指纹图谱方法较HPLC大大缩短了分析时间,可用于金银花药材的质量评价。     

不同产区木瓜药材质量对比分析

目的 考察市售木瓜药材主流商品质量,为木瓜药材商品规格等级标准的建立奠定基础。方法 收集三大主流产区的木瓜样品38批,采用HPLC特征图谱表征其化学成分,运用SPSS软件整体分析特征图谱相似度数据,采用偏最小二乘-判别分析（PLS-DA）特征图谱统计分析,并用正交偏最小二乘-判别分析（OPLS-DA）对宣木瓜和资丘木瓜进行化学成分差异性分析。结果 所建立的木瓜药材特征图谱共有12个共有峰,指认了白桦酸、齐墩果酸、熊果酸、科罗索酸和乙酰熊果酸5个共有峰;直观分析显示宣木瓜和资丘木瓜的特征峰有较大差异,该方法可以有效鉴别宣木瓜和资丘木瓜;特征图谱PLS-DA结果表明不同批次川木瓜存在较大差异,宣木瓜与资丘木瓜之间有显著差异;宣木瓜和资丘木瓜特征图谱OPLS-DA结果表明,二者差异成分峰有峰8（齐墩果酸）、峰9（熊果酸）、峰11、峰3、峰1和峰6（白桦酸）。结论 3个产区木瓜药材化学成分存在显著差异,其中川木瓜品质较差,初步判定宣木瓜优于资丘木瓜。