苦黄注射液中挥发性成分总含量的测定

苦黄注射液是由国家卫生部批准生产的中药复方静脉注射液,属国家二类中药新药。处方由大黄、苦参、茵陈、柴胡等中药组成。具有清热利湿、疏肝褪黄的功能。临床上适用于因湿热内蕴而引起的病毒性黄疸型肝炎患者的退黄。药理研究表明,其挥发性成分为其有效活性成分之一。本文对苦黄注射液中挥发性成分的总含量加以测定,从而对苦黄注射液的质量控制提供了一个科学依据。     

苦黄注射液中乙酸乙酯萃取物成分表征

用薄层分析、熔点测定、质谱、经外、核磁共振方法对苦黄注射液中酯溶性部分（乙酸乙要互可溶性部分）进行了成分分析,共鉴定了5种晶体,它们分别是大黄酚、大黄素甲醚、大黄酸、咖啡酸和没食子酸。     

GC/MS法研究苦黄注射液中挥发油成分

利用气相色谱-质谱联用装置分析了苦黄注射液中挥发油的化学成分及相对含量。共鉴定了55个化合物,其中以单萜和倍半萜为主,占已鉴定的挥发油种类的56．36％和3．63％,为挥发油的主要成分。     

火焰原子吸收光谱法测定苦黄注射液及其中药材中五种金属元素

用硝酸和过氧化氢消化样品，通过基体改进剂，使用火焰原子吸收光谱法测定苦黄注射液及其中药材大黄、茵陈、柴胡、苦参中铜、铁、锌、钾和钠的含量。方法的回收率在92．6％～112．1％之间，相对标准偏差小于4％。     

中药大黄中羟基蒽醌类成分的分离

依据正交试验设计方法,研究了用乙醇和乙醚等溶剂分离中药大黄中羟基蒽醌类成分（蒽甙及游离羟基蒽醌类成分）及游离羟基蒽醌类成分的最佳分离条件,试验表明,乙醇的用量及回流次数对提取产率有很大影响,而回流时间的影响相对较小,100g大黄干粉的最佳分离条件是：用90mL95%乙醇浸润,再用150－175ml乙醇回流,回流3次,每次30－40min,即可较充分发将羟基蒽醌类成分总量的84％及游离羟基蒽醌类成分总量的82％提取出来。     

大黄游离羟基蒽醌的TG-DTA分析

大黄游离羟基蒽醌的TG-DTA分析;大黄;游离羟基蒽醌;热重法（TG）;差热分析（DTA）     

石墨炉原子吸收光谱法测定苦黄注射液及其中药材中的铅和镉

应用石墨炉原子吸收光谱（GF-AAS）法测定了苦黄注射液及其生中药材中铅及镉量。试样用浓硝酸及过氧化氢消解。对仪器的工作条件,包括波长、光谱带宽、灰化温度及原子化温度,作了试验和优化。选用柠檬酸作为基体改进剂,对大黄、茵陈、柴胡、苦参及“苦黄”注射液等试样中的铅及镉量作了测定,分析结果的相对标准偏差均小于4．4％。按标准加入法作了回收率试验,测得值在96%～110％之间。     

梯度加压毛细管电色谱同时分离大黄提取液中5种蒽醌类化合物

建立了同时分离药用大黄提取液中大黄酸、芦荟大黄素、大黄素、大黄酚和大黄素甲醚5种蒽醌类活性成分的梯度加压毛细管电色谱的新方法.实验结果显示,大黄提取液中的5种蒽醌化合物可在22min内完全分离,梯度洗脱微柱液相色谱的柱效为等度洗脱微柱液相色谱的6.63倍,梯度毛细管电色谱的柱效为梯度微柱液相色谱的4.6倍.     

大黄中有效成分的提取、分离测定及其抗突变作用

大黄为常用中药,多年来,对其研究热潮方兴未艾。本文对大黄中有效成分的提取方法,分离和含量测定手段进行了综述,对大黄的抗突变作用进行了论述。     

区带毛细管电泳分离测定大黄提取液中游离蒽醌化合物

采用区带毛细管电泳法分离和同时测定大黄提取液中五种蒽醌化合物的含量。毛细管电泳的分离条件为:50 cm×75μm i.d.未涂层石英分光毛细管,分离电压20kV,0.05 mol/L KH2PO4-Na2HPO4(pH=8.2)缓冲溶液,紫外检测波长为254 nm,以氨基苯磺酸为内标。该法简便,快速,分辨率高,重现性好。     

溶剂浮选法分离富集大黄中的有效成分

采用溶剂浮选法对大黄提取液中的芦荟大黄素、大黄素、大黄酚以及大黄素甲醚进行了分离富集,并用高效液相色谱法分别测定了其含量。考察了料液浓度、浮选溶剂、浮选时间、浮选液pH值、氮气流速和电解质NaCl浓度对浮选效率的影响,并与泡沫浮选法和溶剂萃取法进行了比较。结果表明：溶剂萃取效果最差,泡沫浮选次之,溶剂浮选法分离富集效果最好。当料液浓度为6．4mg／mL,浮选时间为30min,浮选液pH一1～2,氮气流速为20mL／min,电解质NaCl浓度为0．4mol／L时,溶剂浮选效率最佳。     

Temperature-assisted ionic liquid dispersive liquid-liquid microextraction combined with high performance liquid chromatography for the determination of anthraquinones in Radix et Rhizoma Rhei samples

In this article, a novel method termed as temperature-assisted ionic liquid dispersive liquid-liquid microextraction (TA IL-DLLME) combining high performance liquid chromatography with diode array detection (HPLC-DAD) was developed for the determination of anthraquinones in Radix et Rhizoma Rhei samples. The ionic liquid (1-hexyl-3-methylimidazolium hexafluorophosphate) was used to replace volatile organic solvent as an extraction solvent for the extraction of anthraquinones (aloe-emodin, rhein, emodin, chrysophanol and physcion) from Radix et Rhizoma Rhei. Several important parameters influencing the extraction efficiency of TA IL-DLLME such as the type and volume of extraction solvent and disperser solvent, sample pH, extraction time, extraction temperature, centrifugation time as well as salting-out effects were optimized. Under the optimal conditions, the spiked recovery for each analyte was in the range of 95.2-108.5%. The precisions of the proposed method were varied from 1.1% to 4.4% (RSD). All the analytes exhibited good linearity with correlation coefficients (r²) ranging from 0.9986 to 0.9996. The limits of detection for all target analytes were ranged from 0.50 to 2.02 μg L⁻¹ (S/N = 3). The experimental results indicated that the proposed method was successfully applied to the analysis of anthraquinones in Radix et Rhizoma Rhei.     

Classification of Rhizoma et Radix Notoperygii by HPLC Fingerprints with the Aid of Chemometrics

Chromatographic profiles of Rhizoma et Radix Notoperygii (RRN, “Qianghuo” in Chinese), a complex traditional Chinese medicine (TCM), were collected by high-performance liquid chromatography with diode array detection (HPLC-DAD) at 330 nm. These data profiles were used as fingerprints to investigate quality control classification modeling of the RRN samples. In contrast to the classical methods for discrimination of TCMs, that is, just using common HPLC peaks, all chromatographic profile data were pre-processed by the correlation optimized warping method and polynomial functions; then, these data were submitted as fingerprints (variables) for classification on the basis of sample origin. Chemometrics methods used for calibration modeling and subsequent sample classification-least square support vector machine (LS-SVM), artificial neural network (ANN), and partial least square discriminant analysis (PLS-DA); all produced satisfactory calibrations as well as classification results.     

Rapid optimization of dual-mode gradient high performance liquid chromatographic separation of Radix et Rhizoma Salviae Miltiorrhizae by response surface methodology

An approach for rapid optimization of dual-mode gradient high performance liquid chromatography (HPLC) by response surface methodology (RSM) was developed for fast simultaneous separation of hydrophilic and hydrophobic components in Radix et Rhizoma Salviae Miltiorrhizae (Danshen) and its preparations. The aim of this study was to achieve a high throughput RSM optimization using a short ultra-high performance liquid chromatographic (UHPLC) column to simultaneously optimize flow rate and solvent gradient, and then transfer the optimized method to conventional HPLC for routine analytical purposes. The optimization was designed with Box Behnken design (BBD) and the global Derringer's desirability was used for describing the multicriteria response variables. Sixty-two designed experiments were performed by UHPLC with a short sub-2 μm column (2.1 mm × 50 mm, 1.7 μm) and a total running time of only 5 h. The predicted gradient profile was further transferred to a long UHPLC column (2.1 mm × 100 mm, 1.7 μm) and a conventional HPLC columns (2.1 mm × 100 mm, 3.5 μm and 4 mm × 100 mm, 5 μm, respectively). Compared to the published methods, the newly developed dual-mode gradient is faster and more efficient at simultaneously separating hydrophilic and hydrophobic components in Danshen and its preparations.     

Differentiation of Rhizoma Curcumas Longae and Radix Curcumae by a Multistep Infrared Macro-Fingerprint Method

A multistep infrared macro-fingerprint method was applied to identify two Chinese herbal drugs, Rhizoma Curcumas Longae (RCL) and Radix Curcumae (RC). Fourier transform infrared (FT-IR) spectra of the two were similar to each other and consistent with the 11 peaks of the spectrum of starch. RCL had a characteristic absorption peak at approximately 1514 cm^?1 that correlated to the strong peak near 1509 cm^?1 of curcumin. Between 900 cm^?1–1700 cm^?1 of the second derivative infrared (SD-IR) spectra, with higher resolution, RCL, and curcumin had 10 common peaks. In the FT-IR and SD-IR spectra of the ethanol extract, the spectra of the RCL extract and curcumin were similar, but RC was different. According to the fingerprint characteristics of the infrared spectra for RC and its extracts, the strongest peak at 1055 cm^?1; the C-O absorption peaks at 1124 cm^?1, 1106 cm^?1, and 996 cm^?1; and the strong methylene peaks at 2925 cm^?1 and 2853 cm^?1 suggest that RC contains more saccharides. In the range of 1350 cm^?1–1700 cm^?1, RCL and RC had similar two-dimensional infrared (2D-IR) correlation spectra. Both of them had three autopeaks, but the autopeaks were located at 1458 cm^?1, 1560 cm^?1, and 1641 cm^?1 for RCL and 1458 cm^?1, 1560 cm^?1, and 1669 cm^?1 for RC, suggested that the aromatic components of the two were not identical. The average correlation for the 18 RCL and 18 RC samples were 0.9906 and 0.9878, respectively, and this method achieves a good classification of the sample type.     

Separation and identification of the organic acids in Angelicae Radix and Ligustici Rhizoma by HPLC and CE

Angelicae Radix (AR) and Ligustici Rhizoma (LR) are both derived from the Umbelliferae plants and contain similar organic acids as their bioactive compounds. Nine of these organic acids, including nicotinic acid, protocatechuic acid, phthalic acid, folinic acid, p-hydroxybenzoic acid, folic acid, vanillic acid, caffeic acid, and ferulic acid were separated by HPLC and CE. Detection at 210 nm with a linear gradient containing 20 mM KH2PO4 (pH 3.5) and H2O-CH3CN in HPLC and with a buffer solution containing 10 mM LTAC, 2 mM Na2HPO4, 9 mM Na2B4O7(pH 9.56), and CH3CN in CE were found to be the most efficient eluents for this separation. The contents of the nine components in crude extracts of either AR or LR could easily be determined within 60 min by LC and within 20 min by CE. The structures of the individual peaks in the LC chromatogram were identified by LC-MS. The effects of buffers on the separation and validation of the two methods were examined.     

测定天然和栽培缬草根金属元素的微波和干灰化消解-FAAS法

采用微波消化法和马弗炉干灰法处理天然和栽培缬草根样品,火焰原子吸收光谱法连续测定样品中金属元素,分别检出12种和11种元素,其中Zn、Cu、Fe、Co、Mn、Ni、Cr为生命必需微量元素;两种样品各用两种消化法处理,测得金属元素及含量有差异,干灰法操作简单,但消化温度高、时间长、易挥发、元素容易损失,使检测值偏低;而微波消化法简便、省时、损失减少;两种消化法的加标回收率分别为95％-100％和96％-105％。     

野生与栽培羌活药材挥发油含量及组分的比较分析

分析野生和栽培羌活药材挥发油含量及其组分的变化,为羌活药材的引种栽培及进一步的开发利用提供了依据.采用水蒸气蒸馏法提取羌活药材中的挥发油,通过GC-MS对挥发油成分进行分析鉴定;利用聚类分析对测定结果进行分类;通过相关分析研究海拔对羌活药材挥发油含量的影响.6份药材样品挥发油含量范围为1.60～7.98mL/100g,6份羌活药材挥发油成分经GC-MS分析,共鉴定出57个化合物,共有成分12个;基于挥发油成分种类及相对含量的聚类分析显示了羌活药材挥发性成分种类及含量的种间差异;相关分析结果表明,海拔高度与挥发油含量存在显著正相关.野生和栽培羌活药材挥发油含量存在差异,总体上野生羌活药材的挥发油含量高于栽培种;羌活药材挥发油含量随海拔升高而增加.     

反相高效液相色谱法测定大黄药材中游离及结合型蒽醌类衍生物的含量

建立了同时测定大黄药材中蒽醌类衍生物含量的RP HPLC法。色谱柱为HypersilC1 8柱 (2 5 0mm×4 6mmi.d .,1 0 μm) ,流动相为甲醇 乙腈 水 (3∶5∶2 ,磷酸调pH 2 .8) ,流速为 1 .0mL min ,柱温为 2 5℃ ,检测波长为 2 2 5nm。在此色谱条件下 ,各组分在 2 0min内均得到良好分离。平均回收率为 98.83 %～ 1 0 0 .9% ;相对标准偏差 0 .68%～ 1 .5 8%。     

流动注射化学发光法测定曲克芦丁

基于曲克芦丁对Luminol-K_2S_2O_化学发光体系的强烈抑制作用,结合流动注射技术,建立了流动注射化学发光法测定曲克芦丁的新方法.在优化的实验条件下,该法的线性范围为1.0 ×10~(-7)～6.7×10~(-5)mol/L,检出限为8.0×10~(-8)mol/L,对4.0×10~(-7)mol/L曲克芦丁进...