Simultaneous Determination of Three Components in Herba Taxilli from Different Host Trees by HPLC

[Objectives] To establish a HPLC method for the simultaneous determination of three components( namely,quercetin,quercitrin and avicularin) in Herba Taxilli. [Methods]Agilent C18 liquid chromatography column( column size: 150 mm × 4. 6 mm,5 m) was used;mobile phase Dacetonitrile∶ water = 22∶ 78; flow rate: 1. 0 m L/min; column temperature: 35℃; injection volume: 10 μL; detection wavelength: 254 nm. [Results]The injection volume of quercetin,quercitrin and avicularin was in a good linear relationship with the peak area in the range of 0. 22-4. 4 μg( R = 1),0. 096-3. 84 μg( R = 0. 999 6),and 0. 106-5. 3 μg( R = 0. 999 9),and the average sample recovery was 99. 32%,100. 53%,and 98. 96%,respectively. [Conclusions]The stability and reproducibility of the established method for determining the content of Herba Taxilli in this experiment are good,and it is expected to provide reference for its quality control and evaluation.

Rapid HPLC Method for Monitoring Relevant Residues of Pharmaceuticals Products in Environmental Samples

This work presents a multi-residue analytical method based on solid phase extraction (SPE) followed by high-performance liquid chromatographic (HPLC) with diode array (DAD) detection for the simultaneous determination of a group of pharmaceutical products that include ten antidepressants and three anticanceri- genic in environmental samples (water and soil). Baseline separation of the studied compounds was obtained on an ultrabase C18 (4.6 mm i.d. × 150 mm, 5 μm particle) column using acetonitrile:phosphate buffer pH 2.5 (35:65 v/v) as mobile phase with a flow rate of 1.5 mL/min. Different aspects including linearity, accuracy, precision and detection and quantification limits were examined in order to validate the proposed method. Detection limits between 1 and 50 ng/mL were obtained for all the target compounds. This method was ap- plied to the analysis of environmental samples as waters and soils of different precedence. Prior, the HPLC determination the samples were purified and enriched using SPE or liquid-liquid extraction (LLE) of the tar- get compounds.

柑橘果肉、果皮中酚类物质含量差异性研究

采用高效液相色谱法(high performance liquid chromatographic,HPLC)对8种橙类和杂柑中10种酚类物质含量进行测定,探讨不同柑橘品种果肉和果皮中酚类物质种类和含量的差异,分析其规律。结果表明,10种物质能在55 min内分离,线性范围为0.25~200 mg/L,相关系数达0.999 1~1,精密度(RSD≤1.90%)、重复性(RSD≤3.52%)和稳定性(RSD≤4.22%)较好,平均回收率为90.26%~118.85%(RSD为0.96%~3.01%),表明方法的准确度较高。在橙类和杂柑中,橙类果皮中芥子酸含量显著高于杂柑,杂柑果皮中芦丁含量显著高于橙类;果肉中酚类物质含量低于果皮;果实中酚酸以咖啡酸和绿原酸为主,类黄酮以芦丁和柚皮苷为主;在8个柑橘品种果肉中,金诺的阿魏酸、没食子酸和芦丁含量最高。在8个柑橘品种果皮中,口之津32号的咖啡酸、阿魏酸、对羟基苯甲酸含量最高,沃柑的新橙皮苷、柚皮苷、没食子酸和绿原酸含量最高。

Determination of Trace Amount of Polycyclic Aromatic Hydrocarbons in Urban Sewage by Solid-phase Extraction Coupled with High Performance Liquid Chromatograph

[Method] This study aimed to determine trace amount of polycyclic aromatic hydrocarbons(PAHs) in urban sewage by using solid-phase extraction(SPE) coupled with high performance liquid chromatograph(HPLC).[Method] From the aspects of solid-phase extraction column,elution solvent,elution volume,elution speed and so forth,the test conditions of SPE-HPLC method were optimized,and trace amount of PAHs in urban sewage was determined.[Result] The optimized solid-phase extraction conditions were SUPELCLEAN LC-18 solid-phase extraction column,methylene dichloride as elution solvent,15 ml elution volume,2 ml/min elution speed,5 ml/min loading speed,1 000 ml water with 200 ml methanol loading volume.Under the optimized extraction conditions,the recovery was high,namely 76.3%-105.2%;relative standard deviation was 3.8%-6.0%,showing good precision;detection limit was low,only 0.000 8-0.048 0 μg/L.[Conclusion] This method is user-friendly,with high sensitivity and good precision,and suitable for continuous determination of a large volume of water samples.

Freshwater algae chemotaxonomy by high-performance liquid chromatographic(HPLC)analysis

The study of community composition of algae is essential for understanding the structure and dynamics of the aquatic ecosystem and for evaluating the eutrophic level of the water body.A high-performance liquid chromatographic(HPLC)method based on a reversephase C_(18) nonpolar column was developed for the main algal taxa,which includes cyanophytes,bacillariophytes,euglenophytes,dinophytes,and chlorophytes.Based on the elution order using HPLC,19 pigments were identified,and they were chlorophyllide a,19′-butanoyloxyfucoxanthin,chlorophyll c_(1)+c_(2),phephorbides a,peridinin,methyl-chlorophyllide a,fucoxanthin,neoxanthin,violaxanthin,myxoxanthophyll,diadinoxanthin,diatoxanthin,lutein,zeaxanthin,chlorophyll b allomer,chlorophyll b,chlorophyll a allomer,chlorophyll a,andβ,β-carotene.A comparison study of cell microscopic counts and accessory pigment analysis indicated that HPLC analysis could be a useful tool for monitoring phytoplankton communities and their abundance.

Determination of Amantadine Residue in Honey by Solid-phase Extraction and High-performance Liquid Chromatography with Pre-column Derivatization and Fluorometric Detection

Amantadine （AMA） is an anti-viral drug used in apiculture to protect honeybee against the sacbrood virus （Morator aetatulae）. This study described a reliable high-performance liquid chromatographic （HPLC） method for analyzing AMA in honey using a solid-phase extraction （SPE） cartridge （Plexa PCX） for purification, 4-fluoro-7- nitro-2,1,3-benzoxadiazole （NBD-F） as a pre-column derivatization agent, and fluorometric detection （λex =470 nm, λem=530 nm）. The chromatographic separation was performed on an XDB C18 column （150×4.6 mm i.d.） using 0.1% trifluoroacetic acid/acetonitrile （35 ; 65, V/V） as the mobile phase at a flow rate of 1.0 mLomin 1 with a run time of 20 min. Under these optimal conditions, a linear relationship was observed in the range of 0.025--1.0μg·mL-1 with a good correlation coefficient （0.998） and low limit of detection （0.0080 μg·g-1）, the recoveries were all above 90%, and the intra-day and inter-day precision （RSD） ranged from 3.4%--5.1%.

Determination of Ciprofloxacin in Human Plasma and Urine by Precolumn Derivatization High Performance Liquid Chromatography with Fluorescence Detection

A sensitive, simple and selective high-performance liquid chromatographic （HPLC） method was developed for the determination of ciprofloxacin in biological fluids. The method is based on the reaction between the drug and 4-chloro-7-nitrobenzofurazan （NBD-C1） in borate buffer of pH 9.0 to yield a highly fluorescent derivative that is measured at 535 nm after excitation at 464 nm. The calibration curves were linear over the concentration ranges of 25--3000 and 50--3000 ng·mL -1 for plasma and urine, respectively. The mean recovery of ciprofloxacin from plasma and urine was 98.37% and 98.40%, respectively. The method was found to be sensitive, precise, accurate, and reproducible. All of the validation parameters were within the acceptance range.

Control System for Low Pressure Gradient Mixer in High Performance Liquid Chromatograph

A control system used in high performance liquid chromatograph(HPLC) was described.The control system adopting low pressure gradient elution was tested with different initial and end volume fractions,and four types of gradient elution curves.The experimental results verified the theoretical analyses of the applied method.This self-designed control system can achieve approving accuracy,repeatability and low cost,which has a bright outlook for domestic applications.