Establishment of Characteristic Chromatogram of Honeysuckle Stem Formula Granules Based on the Concept of Whole Process Quality Control

[Objectives]To establish a HPLC characteristic spectrum of honeysuckle stem formula granules,and to evaluate the quality consistency based on the standard decoction.[Methods]Using Agilent ZORBAX SB-C_(18)(5μm,250 mm×4.6 mm)chromatographic column;gradient elution with acetonitrile-0.4%phosphoric acid solution(0.2:99.8,V/V),column temperature at 25℃;detection wavelength at 236 nm;flow rate 1.0 mL/min;using"Similarity Evaluation System for Chromatographic Fingerprint of Traditional Chinese Medicine",to evaluate the similarity of the characteristic chromatogram of crude drug,standard decoction and formula granules of honeysuckle stem.[Results]The similarity of characteristic chromatogram was higher than 0.94,and 6 components were identified from 10 characteristic peaks.[Conclusions]The established method can more comprehensively reflect the overall appearance of the chemical substances in the honeysuckle stem and the transmission law,and can provide an experimental basis for the consistency of the quality of the honeysuckle stem formula granules.

Bohai crude oil identification by gas chromatogram fingerprinting quantitative analysis coupled with cluster analysis

By gas chromatogram, six crude oils fingerprinting distributed in four oilfields and four oil platforms were analyzed and the corre- sponding normal paraffin hydrocarbon （ including pristane and phytane） concentration was obtained by the internal standard methed. The normal paraffin hydrocarbon distribution patterns of six crude oils were built and compared. The cluster analysis on the normal paraffin hydrocarbon concentration was conducted for classification and some ratios of oils were used for oils comparison. The results indicated： there was a clear difference within different crude oils in different oil fields and a small difference between the crude oils in the same oil platform. The normal paraffin hydrocarbon distribution pattern and ratios, as well as the cluster analysis on the nomad paraffin hydrocarbon concentration can have a better differentiation result for the crude oils with small difference than the original gas chromatogram.

Identification of three kinds of Plumeria flowers by DNA barcoding and HPLC specific chromatogram

DNA barcoding and HPLC specific chromatogram were used to identify three kinds of Plumeria flowers respectively. DNAs extracted from the three Plumeria species were amplified by PCR with universal primers, and the psbA-trnH region was selected. All the amplified products were sequenced and the results were analyzed by MEGA 5.0. Chemometric methods including principal components analysis and hierarchical clustering analysis were conducted on the SAS 9.0 software to demonstrate the variability among samples. In conclusion, the psbA-trnH of all samples were successfully amplified from total DNA and sequenced. These three varieties of Plumeria can be differentiated by the psbA-trnH region and clustered into three groups respectively through building neighbor joining tree, which conformed to their germplasm origins. However, it was hard to distinguish them by HPLC specific chromatograms combined with chemometrics analysis. These indicated that DNA barcoding was a promising and reliable tool for the identification of three kinds of Plumeria flowers compared to HPLC specific chromatogram generally used. It could be treated as a powerful complementary method for traditional authentication, especially for those varieties which are difficult to be identified by conventional chromatography.

Identification of HPLC Characteristic Chromatograms of Phenylethanoid Glycosides and Iridoid Glycosides in Herba Cistanche of Different Origins

[Objectives]This study aimed to establish a quality evaluation method for Herba Cistanche based on the HPLC characteristic chromatograms of the phenylethanoid glycosides and iridoid glycosides,and compare the HPLC characteristic chromatograms of different origins of Herba Cistanche.[Methods]The chromatographic conditions used were as follows:column,Agilent ZORBAX Eclipse Plus C18 column(4.6 mm×250 mm,5μm);gradient elution,acetonitrile-0.1%phosphoric acid aqueous solution;flow rate,1.0 mL/min;detection wavelength,240 nm;column temperature,30℃.[Results]Cistanche tubulosa(Schenk)Wight showed 9 characteristic peaks,Cistanche deserticola Y.C.Ma showed 10 characteristic peaks,Cistanche salsa(C.A.Mey.)G.Beck showed 7 characteristic peaks,and Cistanche sinensis G.Beck showed 4 characteristic peaks.Peak 6 was echinacoside,peak 7 was verbascoside,peak 8 was tubuloside A,peak 9 was isoacteoside and peak 10 was cistanoside A.The characteristic chromatograms of the four different origins of Herba Cistanche were significantly different.[Conclusions]This characteristic chromatogram method has good reproducibility and can be used to distinguish 4 different origins of Herba Cistanche,C.deserticola Y.C.Ma,C.tubulosa(Schenk)Wight,C.sinensis G.Beck and C.salsa(C.A.Mey.)G.Beck.

HPLC Fingerprint Chromatogram of Tetracera asiatica Produced in Guangxi

[Objectives] To establish fingerprint chromatogram of Tetracera asiatica and provide basis for controlling and assessing the quality of Tetracera asiatica.[Methods] The high-performance liquid chromatography( HPLC) method was used. Phenomenex C18( 5 μm,4. 6 ×250 mm),acetonitrile-0. 1% phosphoric acid water,gradient elution,flow rate 1 m L/min,detection wavelength 214 nm,and column temperature 25 ℃. The fingerprint chromatogram of 10 batches of samples of Tetracera asiatica was determined for similarity comparison. [Results] It established HPLC fingerprint chromatogram of Tetracera asiatica produced in Guangxi,determined a total of 13 common fingerprint peaks. The similarity of 10 batches of Tetracera asiatica was > 0. 9.[Conclusions] The method is rapid and accurate and can provide references for assessing the quality of Tetracera asiatica.

Establishment of Specific Chromatogram of Spica Prunellae Formula Granules Based on Standard Decoction

[Objectives]This study aimed to establish HPLC chromatograms of decoction pieces,standard decoction and formula granules of Spica Prunellae.[Methods]The chromatographic conditions were as follows:column,SHISEIDO CAPCELL PAK C18 MGII column(4.6 mm×250 mm,5μm);mobile phase,acetonitrile-0.1%phosphoric acid;gradient elution;detection wavelength,280 nm;flow rate,1.0 mL/min;and column temperature,30℃.The correlation between the decoction pieces,standard decoction and formula granules of Spica Prunellae was analyzed by specific chromatograms.[Results]The fingerprint chromatograms of decoction pieces,standard decoction and formula granules of Spica Prunellae showed five common peaks,with good correlation.Among the five common peaks,four of them were tanshinol,protocatechuic acid,caffeic acid and rosmarinic acid.[Conclusions]The main chemical constituents of decoction pieces,standard decoction and formula granules of Spica Prunellae are basically the same.The HPLC specific chromatogram established can be used for the quality control of Spica Prunellae formula granules.

Typical HPLC Chromatogram of Petroleum Ether in Abutilon indicum(L.) Sweet from Different Habitats

[Objectives] To study the typical HPLC chromatogram of petroleum ether in Abutilon indicum (L.) Sweet from different habitats, in order to provide experimental basis for the quality control of A. indicum and the spectrum-efficacy relationship of petroleum ether.[Methods] The HPLC chromatogram of petroleum ether was obtained using Agilent SB-C 18 (4.6 mm×250 mm, 5 μm) and acetine-0.1% phosphoric acid solution for gradient elution at temperature of 30 ℃, flow rate of 1.0 mL/min and detection wavelength of 205 nm.[Results] The typical HPLC chromatogram of petroleum ether in A. indicum was preliminarily established, with 12 characteristic peaks. It was verified by A. indicum from different habitats, characterized by reproducibility and stability.[Conclusions] Typical HPLC chromatogram provides a stable new method for the quality control of petroleum ether in A. indicum . This study provides experimental basis for further study on the medicinal parts of A. indicum .

Analysis for the Defect of Chromatogram in 35kv Oil-immersed Electric Reactor

A defect of chromatogram in a 35kV oil-immersed three-phase one-piece electric reactor in a 500kV substation。The initial analysis suggests that the defect is caused by the loose connection of the iron core magnet shield (magnet shield layer of iron core or earthling top). Examination of winding DC resistance, DGA and other relevant examinations were carried out to investigate the defect reasons., which is demonstrated by the dismantlement. In-depth study is taken and corresponding prevention measures are put forward in the paper.

Study on the Specific GC Chromatograms of Volatile Oil from Xinyi Biyan Pills

[Objectives]This study was conducted to establish characteristic chromatograms of of the volatile oil of Xinyi Biyan Pills by gas chromatography,discover possible problems in the production processes of different manufacturers,and further improve the quality control methods.[Methods]The volatile oil in samples was extracted and tested by gas chromatography to collect chromatograms,which were analyze and evaluated by the similarity evaluation software of chromatographic fingerprints of traditional Chinese medicine.[Results]Nineteen common peaks were calibrated in the characteristic chromatograms;and the characteristic chromatograms of samples produced by different manufacturers were obviously different.[Conclusions]Controlling the volatile components in Xinyi Biyan Pills by the established characteristic chromatograms of GC is accurate and feasible,and can be used as a quality control method for Xinyi Biyan Pills.

Research on Comparison of Gas Chromatography and Liquid Chromatogram Detecting Pesticide Residue

The existing methods of detecting pesticide residue include gas chromatography, high performance liquid chromatography, gas chromatograph-mass, liquid chromatograph-mass, capillary electrophoresis, radioimmunoassay, biosensor and rapid detection on the spot. The paper analyzes the comparison of gas chromatography and liquid chromatogram detecting pesticide residue, for achieving the development tendency and the future goal of analyzing pesticide residue.

基于UPLC特征图谱和含量测定的蜜远志标准汤剂质量评价研究

目的建立蜜远志标准汤剂特征图谱以及3种成分质量分数同时测定的UPLC方法,对不同来源蜜远志饮片制成的标准汤剂质量进行评价。方法采用UPLC法建立蜜远志标准汤剂的特征图谱以及细叶远志皂苷、远志酮Ⅲ和3,6′-二芥子酰基蔗糖质量分数测定的方法,并对16批标准汤剂进行测定,采用高分辨质谱对共有峰进行了指认,采用聚类分析及偏最小二乘法分析(PLS-DA)对共有峰进行了分析。结果蜜远志标准汤剂特征图谱标定了9个共有峰,通过高分辨质谱分别指认为:西伯利亚远志糖A5、西伯利亚远志糖A6、远志酮Ⅲ、3,6′-二芥子酰基蔗糖、黄花远志素A、细叶远志皂苷A、远志寡精H、远志寡糖A、1,2,3,7-四甲氧基呫吨酮,相似度结果显示16批样品的相似度均大于0.900。聚类分析及PLS-DA显示不同来源之间的样品可能存在质量差异。结论本研究建立的蜜远志标准汤剂特征图谱和质量分数测定方法简便、快速、准确,可为蜜远志相关制剂的质量评价提供参考。

瑶药小钻的特征图谱及其安五脂素含量和抗炎活性研究

目的 建立瑶药小钻特征图谱及其主要成分安五脂素含量测定方法,并评价安五脂素抗炎活性。方法 采用高效液相色谱法,以乙腈-0.5%磷酸溶液为流动相进行梯度洗脱,采用《中药色谱指纹图谱相似度评价系统(2012版)》建立小钻药材的特征图谱和进行相似度评价,并测定小钻中安五脂素含量。以脂多糖诱导的RAW264.7巨噬细胞为炎症细胞模型,考察安五脂素对细胞上清液中肿瘤坏死因子α(TNF-α)、白细胞介素1β(IL-1β)、IL-6水平的影响。结果 10批小钻样品的特征图谱相似度为0.901~0.994;标定了9个共有峰,指认了3个成分,分别为长南五味子素E、南五味子内酯A、安五脂素;安五脂素的含量为(0.72±0.05)~(1.21±0.03)mg/g(n=3)。0.125~0.5μg/mL的安五脂素可显著降低炎症模型细胞上清液中TNF-α、IL-1β、IL-6水平(P<0.05或P<0.01)。结论 建立了小钻药材HPLC特征图谱及其安五脂素含量测定方法;安五脂素可能是小钻药材发挥抗炎作用的有效成分。

清脂化瘀方HPLC-CAD特征图谱建立及6种糖类含量测定

目的建立清脂化瘀方HPLC-CAD特征图谱,并测定鼠李糖、果糖、甘露醇、D-无水葡萄糖、蔗糖、棉子糖的含量。方法分析采用Dikma Polyamino HILIC色谱柱(4.6 mm×250 mm,5μm);流动相乙腈-水,梯度洗脱;体积流量0.8 mL/min;柱温35℃。结果15批样品特征图谱中有14个特征峰相似度大于0.90。6种糖类在各自范围内线性关系良好(r>0.9950),平均加样回收率93.34%~105.64%,RSD 0.5%~2.6%。结论该方法准确可靠,灵敏度高,重复性好,可用于清脂化瘀方糖类的质量控制。

溶剂提取-高效液相色谱法测定大气颗粒物中18种多环芳烃

建立大气颗粒物PM2.5中18种多环芳烃的样品快速溶剂提取结合高效液相色谱的测定方法。将1/2玻璃滤膜剪碎后加入2.0 mL乙腈,于20℃水浴超声提取30 min,提取液经0.22μm有机相滤膜过滤,多环芳烃C18专用柱分离,以乙腈-水作为流动相进行梯度洗脱,采用紫外串联荧光检测器-高效液相色谱仪检测,以色谱峰面积外标法定量。18种PAHs的质量浓度在0.01~0.50μg/mL范围内与色谱峰面积线性关系良好,相关系数不小于0.999,检出限为0.03~0.47 ng/m^(3),样品加标平均回收率为75.6%~114.7%,相对标准偏差为0.09%~3.78%(n=7)。该方法简便、快速、准确、灵敏,可应用于大气颗粒物PM2.5中18种多环芳烃的测定。

CHROMATOGRAM BASE IN EXPERT SYSTEM FOR LIQUID CHROMATOGRAPHY

Ⅰ. INTRODUCTION In the last few years, much effort has been devoted to developing the expert system for liquid chromatography (ESLC). In our previous papers, a strategy for the development of ESLC was established. Establishment of a chromatogram base is one of the most important aspects in developing ESLC. Due to the fact that one of the most time-consuming and often frustrating jobs in chromatographic lab is to develop LC method for a

巴芪柔肝方基准样品HPLC特征图谱建立及其量值传递规律研究

目的建立巴芪柔肝方基准样品HPLC特征图谱,并考察其量值传递规律。方法测定毛蕊异黄酮葡萄糖苷、橙皮苷、迷迭香酸、莪术烯醇、耐斯糖含量,计算饮片-水煎液-基准样品转移率,记录出膏率、pH值。结果15批基准样品HPLC特征图谱中有16个特征峰,相似度均大于0.90,鉴定出9个。饮片-基准样品中耐斯糖、毛蕊异黄酮葡萄糖苷平均转移率分别为(83.14±6.25)%、(77.81±8.31)%,水煎液-基准样品中迷迭香酸、莪术烯醇平均转移率分别为(81.71±6.27)%、(72.16±5.91)%,平均出膏率为(38.91±1.46)%,pH值为5.13±0.08。结论该方法稳定可行,可为巴芪柔肝方制剂工艺选择、关键化学属性评价提供参考。

基于电子鼻和气相色谱技术筛选石菖蒲的质量标志物

采用PEN3电子鼻系统分析不同批次石菖蒲挥发油气味信息,并进行雷达图分析、Loading分析和主成分分析处理;采用气相色谱分析挥发油中主要化学成分含量,并对气味值和主要化学成分含量进行相关性分析,筛选其质量标志物。电子鼻气味分析系统结果显示,21批石菖蒲挥发油整体气味信息主要体现在W5S、W1W和W2W上;气相色谱分析结果显示挥发油中β-细辛醚含量最高,α-细辛醚次之;相关性分析中β-细辛醚与W2W具有显著的正相关关系,因此电子鼻结合气相色谱技术可以用来评价石菖蒲药材质量,β-细辛醚可作为石菖蒲的质量标志物。

HPLC特征图谱技术在中药制剂质量控制中的应用进展

高效液相色谱特征图谱技术具有整体性的特点,与中药复杂的化学成分特征相符,已被国内外公认为中药质量控制的良好方法之一,是表征中药制剂质量和保证中药制剂临床疗效的重要手段。本文综述了近年高效液相色谱特征图谱技术在中药制剂质量控制中的应用特点,为持续提升中药制剂质控水平提供参考。

清上蠲痛汤标准汤剂挥发油的UPLC特征图谱建立及成分分析

目的建立清上蠲痛汤标准汤剂挥发油的特征图谱,初步推断该方中影响临床治疗效果的主要挥发油类活性成分。方法采用水蒸气蒸馏法提取清上蠲痛汤标准汤剂中挥发油,采用《中药色谱指纹图谱相似度评价系统(2012版)》建立15批样品的超高效液相色谱(UPLC)特征图谱并进行相似度评价;采用超高效液相色谱四极杆飞行时间串联质谱(UPLC-Q-TOF/MS)法对标准汤剂挥发油类成分进行指认、鉴定;采用气质联用(GC-MS)法分析其挥发油类成分组成。结果15批清上蠲痛汤标准汤剂挥发油的UPLC特征图谱的相似度在0.949~0.997之间;共得到12个共有峰,经UPLC-Q-TOF/MS鉴定主要成分为甲基丁香酚、E-藁本内酯、E-正丁烯基苯酞等。GC-MS共鉴定出23个成分,主要为3,4,5-三甲氧基甲苯、百秋李醇、Z-藁本内酯等。结论建立了清上蠲痛汤标准汤剂挥发油的特征图谱,初步推断甲基丁香酚、藁本内酯、E-正丁烯基苯酞、百秋李醇、3,4,5-三甲氧基甲苯可能是影响清上蠲痛汤挥发油临床治疗效果的主要活性成分。

三门峡多油分烟叶有机酸气相指纹图谱的建立

【目的】建立三门峡多油分烟叶的有机酸气相(GC)指纹图谱,明确多油分烟叶的质量特性,为多油分烟叶的质量评价提供参考。【方法】采用硫酸-甲醇法提取多油分烟叶有机酸,通过气相色谱进行分析,获取烟叶样品的色谱图,结合中药指纹图谱相似度评价软件建立多油分烟叶有机酸气相指纹图谱,并进行样品相似度评价;选取云南和湖北的多油分烟叶对所建立的对照图谱进行验证。【结果】三门峡多油分烟叶的指纹图谱有12个有机酸共有峰,分别为草酸、丙二酸、γ-戊酮酸、丁二酸、苹果酸、2,4-庚二烯酸、柠檬酸、十六酸、十七酸、油酸、亚油酸、十八酸。24批样品的有机酸图谱与对照指纹图谱的相似度在0.995~0.999,各批次间样品相似度较好。指纹图谱验证结果表明,三门峡多油分烟叶与云南、湖北等地烟叶之间差异较大。【结论】建立的三门峡多油分烟叶有机酸气相指纹图谱方法简便、可靠、专属性强。