Determination of Benzo[a]pyrene in Edible Oil by High Performance Liquid Chromatography-Fluorescence Detector (HPLC-FL)

In this study, an optimized high performance liquid chromatography-fluorescence detector (HPLC-FL) method for the determination of benzo[a]pyrene in edible oil was established. HPLC was performed with Thermo Fisher Scientific C18 column (250 mm×4.6 mm, 5 μm) as the chromatographic column and acetonitrile and water as the mobile phase, and the excitation wavelength and emission wavelength of fluorescence detector were 286 and 430 nm, respectively. The response was high, and the linear range was 0.5-10.0 ng/ml. The lowest limit of detection was 0.11 ng/ml, and the average recovery was 92.5%. This method is suitable for quantitative analysis of benzo[a]pyrene content in edible oil.

Development of Quantitative Analysis Method of Carbendazim in Tomatoes by High-Performance Liquid Chromatography with Fluorescence Detection(HPLC-FLD)

Carbendazim belongs to the benzimidazole fungicides,which can be used for control lots of fungi pathogens.High-performance liquid chromatography is frequently used for the analysis of carbendazim in all kinds of samples.In most occasions,the developed methods were applied for the simultaneous detection of a huge number of pesticides.Thus,an analytical method via UPLC-FLD was developed,and the sample preparation process was optimized by studying the effect of extraction solvent,approach,time and purification absorbent on the recovery rate of carbendazim.The results showed the optimized method for analysis was ultrasonication-assisted extraction with acetonitrile for 1 min,and subsequent purification by C18.In this occasion,the established analytical method of carbendazim in tomato samples displayed good linearity,accuracy and precision.

Using cell membrane chromatography and HPLC-TOF/MS method for in vivo study of active components from roots of Aconitum carmichaeli

An offline two-dimensional system combining a rat cardiac mascle cell membrane chromatography time-of-flight mass spectrometry （CMC-TOF/MS） with a high performance liquid chromatography time-of-flight mass spectrometry （HPLC-TOF/MS） was established for investigating the parent components and metabolites in rat urine samples after administration of the roots of Aconitum carmichaeli. On the basis of the analysis of the first dimension, retention components of the urine sample were collected into 30 fractions （one fraction per minute）. Then offline analysis of the second dimension was carried out. 34 compounds including 24 parent alkaloids and 10 potential metabolites were identified from the dosed rat urine, and then binding affinities of different compounds on cell membranes were compared and influences of some functional groups on activity were estimated with the semi-quantification and curve fitting method. As a result, binding affinities decreased along with the process of deacylation, debenzoylation and demethylation, which may be related to the alleviation of toxicity in the procedure of herb processing or metabolism. Moreover, some minor components in rat urine （Songorine, 14-benzoylneoline, Deoxyaconitine, etc. ） exerted relatively strong affinity on cell membranes are worth exploring. The results delivered by the system suggest that the CMC can be applied to in vivo study.

Determination of 5-Fluorouracil in Human Plasma by High-Performance Liquid Chromatography (HPLC)

5-Fluorouracil (5-FU) has a broad spectrum of anti-tumor activity, widely applied to the treatment of cancers. However, it is necessary to determine the plasma concentration of 5-FU in clinical practice due to its narrow therapeutic index. Therefore, a simple, economic and sensitive high-performance liquid chromatography (HPLC) method was developed and validated for the determination of 5-FU in human plasma. Ethyl acetate was chosen as extraction reagent. Chromatographic separation was performed on a Diamonsil C18 column (250 mm × 4.6 mm i.d., 5 μm) with the mobile phase consisting of methanol and 20 mmol/L ammonium formate using a linear gradient elution at a flow rate of 0.8 mL/min. 5-FU and 5-bromouracil (5-BU) were detected by UV detector at 265 nm. The calibration curve was linear over the concentration range of 5—500 ng/mL and the correlation coefficient was not less than 0.992 6 for all calibration curves. The intra- and inter-day precisions were less than 10.5% and 4.3%, respectively, and the accuracy was within ±3.7%. The recovery at all concentration levels was 80.1±8.6%. 5-FU was stable under possible conditions of storing and handling. This method is proved applicable to therapeutic drug monitoring and pharmacokinetic studies of 5-FU in human.

Modernization of Chinese herbal compound and the high performance liquid chromatography tandem mass spectrometry (HPLC-MS)

Chinese herbal compound is playing an important role on curing human diseases.And it has been a trend that Chinese herbal compound is being used all over the world in 21 century.However,our Chinese herbal compound is facing serious challenge for the lack of canonical system of quality criterion for Chinese herbal compound so it has been a urgent problem to set up the quality control standards and reveal therapeutic basis of Chinese herbal compound.In order to give full play to the advantages of Chinese herbal compound,modern scientific and technological is used to research of Chinese herbal compound,especially the high performance liquid chromatography tandem mass spectrometry(HPLC-MS),because it is high sensitive,rapid,and obtain more information.It is very necessary that HPLC-MS is uesed to elucidate the effective components of basic substances of Chinese Herbal Compound,and endow traditional Chinese medicine with modern scientific connotation.

Separation of Ephedrines Using 1-Butyl-3-methylimidazolium-tetrafluoroborate Ionic Liquids as Eluent in High-performance Liquid Chromatography (HPLC)

A simple, effective HPLC method for separation of ephedrines was achieved by using 1-butyl-3-methylimidazolium-tetrafluoroborate ionic liquid solution (0.1% v/v) as eluent at pH 3.0. The involved mechanism may be due to that the imidazolium cations can effectively shield the silanol groups of alkylsilica surface, thereby decreasing band tailing and increasing the separation efficiency.

Simultaneous Determination of Sulfamonomethoxine Sodium and Trimethoprim in Compound Sulfamonomethoxine Sodium Propolis Solution by High Performance Liquid Chromatography(HPLC)

[Objective] The paper aimed to provide a basis for quality control of compound sulfamonomethoxine sodium propolis solution. [Method] High per- formance liquid chromatography （HPLC） method was used to determine the contents of sulfamonomethoxine sodium and trimethoprim simultaneously in compound sulfamonomethoxine sodium propolis solution. [Result] Sulfamonomethoxine sodium and trimethoprim showed a linear relationship within the concentration of 10 - 500 μg/mL under the following chromatographic conditions： Kromasil C18 column （250 mm × 4.6 mm, 5 μm）, mobile phase 0.02 mol/L phosphoric acid solution- methanol（80：20, V/V）, detection wavelength 270 nm, flow rate 1.0 mL/min, and column temperature 30℃. The average recoveries were 99.3% and 99.4%, respectively. [ Conclusion] The method is accurate and feasible, and can determine sulfamonomethoxine sodium and trimethoprim simultaneously in compound sul- famonomethoxine sodium propolis solution.

Determination of AF and AFG in Red Ginseng by High Performance Liquid Chromatography with Evaporative Light Scattering Detector (HPLC-ELSD)

[Objective]The paper was to establish a method for determining AF and AFG in red ginseng.[Method]A new simple,rapid and sensitive method for simultaneous determination of two amadori compounds,arginyl-fructose(AF)and arginyl-fructosyl-glucose(AFG),in extracts of three kinds of ginseng preparations was developed and validated using high performance liquid chromatography with evaporative light scattering detector(HPLC-ELSD).Two target analytes were efficiently separated by Prevail CTM18 column(4.6 mm×250 mm,5μm)at the flow rate of 0.8 mL/min within 15 min of single chromatographic run.[Result]Under optimized conditions,the detection limits were 0.015 and 0.02 mg/mL for AF and AFG,respectively.Calibration curves of peak area for two analytes were linear over three orders of magnitude with the correlation coefficients greater than 0.999.The average recoveries,precision,reproducibility and stability for two analytes(AF and AFG)were 99.5% and 100.9%,0.43% and 0.47%,0.46% and 0.43%,0.41% and 0.49%,respectively.[Conclusion]This method was successfully applied for quantifying AF and AFG in red ginseng and the method was efficient,sensitive and accurate.

Analysis of Amino Acids in Houttuynia Cordata Thunb. by High Performance Liquid Chromatography-Diode Array Detector (HPLC-DAD)

[Objectives] The biologically active compounds of Houttuynia cordata Thunb. as a medicinal and edible plant are well documented. However, amino acid as an important indicator of the value of H. cordata is little reported. [Methods] Amino acids of the H. cordata were analysed by pre-column derivatization with 2,4-dinitrochlorobenzne(CDNB) coupled to HPLC/DAD. The optimized conditions of the amino acids derivatized by CDNB were followed: 110 ℃ of hydrolysis temperature, 1∶12 of the equivalent proportion between amino acid and CDNB, 80 min of derivatization reaction time and 80 ℃ of derivatization reaction temperature. The method was used to determine the amino acids of H. cordata samples from 11 different geographical sites in Guizhou. [Results] The results suggested that the contents of 17 amino acids were quite variable at different H. cordata samples. [Conclusions] This study will provide a basis for the quality evaluation of H. cordata nutrition.

Sensitive and Rapid Quantification of Felodipine by High-performance Liquid Chromatography-tandem Mass Spectrometry(HPLC-MS/MS) and Its Pharmacokinetics in Healthy Chinese Volunteers

To investigate the pharmacokinetics of felodipine in the plasma of healthy Chinese volunteers, 30 healthy volunteers received a single oral dose of 5 mg of extended release felodipine tablets. The felodipine was extracted from the matrix with a liquid-liquid extract procedure and analyzed by high-performance liquid chromatography-tandem mass spectrometry in the multiple reaction monitoring（MRM） mode using an electrospray ion source with positive ion detection. The method was validated over a felodipine concentration range of 0. 05-10.00 ng/mL in human plasma. Its main pharmacokinetic parameters values were： ρmax = （ 1.67 ± 0. 84 ） ng/mL, occurring at （ 3.93 3± 2. 49 ） h; the plasma elimination half-life： （23. 08 3± 9. 48） h and the area under the plasma concentration versus time curve： （29. 94 ± 14. 39） ng · h/mL. The validation results demonstrated that this method showed a satisfactory precision and accuracy across the calibration range. The procedure involved minimal drug administration, sample preparation, and a 2. 5-min chromatographic run time. It was well suited to clinical studies of the drug involving large numbers of samples.

The New Type of Liquid Chromatography—Colloidal High-Performance Liquid Chromatography (CHPLC): Further Applications

The recent paper by I. Brondz (2018), “One-Step Procedure for Direct Purification of Pediocin-Like Bacteriocins and Cationic Antimicrobial Peptides from Complex Culture Medium on an Analytical, Semipreparative, and Preparative Scale. A New Type of Liquid Chromatography—Colloidal High-Performance Liquid Chromatography (CHPLC)” (International Journal of Analytical Mass Spectrometry and Chromatography, 6, 41-49, https://doi.org/10.4236/ijamsc.2018.63004), described a new type of CHPLC. This technique allows colloidal liquids and suspensions to be chromatographed directly despite the presence in the liquids of material such as bacteria, fungi, and other soft and hard particles. The significance of this development lies in enabling the single-step cleanup and concentration of the target substance from a complex mixture of soluble molecules in the presence of insoluble particles by high performance liquid chromatography (HPLC). The technique also allows the use of viscose liquids (as described in Brondz (2018) that are not suitable for analysis by conventional HPLC. In the previous paper, emphasis was placed on describing the applications of the techniques for the preparation of target substances such as small peptides, bacteriocins, bacitracin, and lysosome. Normally, the industrial preparation of these substances requires multistep procedures, which are time- and labor-consuming, and typically results in significant loss of target material and specific activity. In the present paper, the application of CHPLC for the isolation of alkaloids from crude raw material such as opium cake is demonstrated. In the opium cake, large amounts of hard vegetable particles and even sand corns are present together with the target alkaloids. Despite this, isolation by CHPLC of the desired compound was achieved in a single step by using a water/ethanol-based liquid. Isolation of alkaloids from such raw material normally requires a multistep procedure that includes the preparation of insoluble tartrate or picrate complex and this process includes dissolving the substance in flammable organic liquid. The isolation described here was performed in a single step by using the water/ethanol-based liquid.

Determination of Capsaicin and Dihydrocapsaicin in Capsicum( Capsicum annuum) Products by High Performance Liquid Chromatography-Fluorescence Detection( HPLCFLD)

[Objectives] This study was conducted to determine capsaicin and dihydrocapsaicin in capsicum products. [Methods]The sample was ultrasonically extracted with anhydrous ethanol as the extraction solvent for capsaicin and dihydrocapsaicin,followed by centrifugation. The extract was subjected to HPLC separation with methanol-water( 65∶ 35) as the mobile phase,and a fluorescence detector( Ex = 229 nm,Em = 320 nm) was used to detect capsaicinoids in the sample. [Results] Capsaicin and dihydrocapsaicin had a good linear relationship in the range of 1-200 mg/L( R_1~2= 0. 999 8,R22= 0. 999 6). The detection limits were both 0. 007 mg/kg; the quantification limits were both 0. 02 mg/kg; the precision was 0. 235% and 0. 754%,respectively; and the average recoveries were95. 94% and 95. 39%,respectively. [Conclusions]The method is simple,rapid,with good sensitivity and precision,and is suitable for detecting capsaicin substances in capsicum products.

DEGRADATION OF LINEAR ALKYLABENZENE SULFONATE(LAS)AND ITS COMPOUNDS IN DONGHU LAKE(HUBEI,P.R.C.)DETERMINED BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY(HPLC)

Commercial linear alkylbenzene sulfonate (LAS), mixture of alkylchain lengths and phenyl position isomers (C10-C13), is widely used as a major constituent of household and industrial detergents in the People’s Republic of China. Degradation process and behaviour of LAS compounds during an 82-hour lake water die-away study, with an added LAS concentration of 1. 5mg .L-1, was quantified and accomplished by HPLO-UV after extractionon the SepPek C18 reversed - phase cartridges. The degradation rate became progressively faster with increasing chain length. The technique described in this study is fast, sensitive and specific, and can be used to determine low levels, of LAS and for establishing water quality criteria and standards relating to LAS and its compounds.

Analysis of Pesticide Raid^(█) in Feed of Wistar Rat by High-Pressure Liquid Chromatography (HPLC)

The distribution of pesticide by-product in tissues of wistar rats were analyzed using high pressure liquid chromatography. The limit of detection of the HPLC was 0.1 μg. Results show bioaccumulation factor of pesticide “Raid?” in lipid, up to three times that of the feed at the first concentration and gradually decreased as the concentration increased in the muscle > (0.7), brain > (0.5) and liver > (0.3) as indicated in the text. At higher concentration of 961 μg/g, bioaccumulation factor decreased in the lipid to 1.2 and 0.6 in the muscle, 0.03 in the brain and 0.08 in the liver respectively. High Pressure Liquid Chromatography (HPLC) analysis of raid extract suggests the presence of micprothrin and palethrin. The implications are numerous, but simply put that accidental ingestion of chlorinated hydrocarbon as in “Raid?” may involve convulsions, collapse and coma after only brief excitation and ataxia at the onset.

High Performance Liquid Chromatography （HPLC）-A Rapid Method of Detecting Melamine in Raw Milk

Project name： GB/T 22400--2008 High Performance Liquid Chromatography （HPLC） -A Rapid Method of Detecting Melamine in Raw Milk

影响HPLC在食品检测中准确性的因素及控制对策

为了提高高效液相色谱法(High Performance Liquid Chromatography,HPLC)在食品检测中的准确性,本文分析了样品前处理、仪器设备、检测人员和实验室环境等因素对检测结果的影响。分析认为,样品前处理不当、仪器设备老化、人员操作不规范以及环境条件不稳定是导致检测不准确的关键因素。针对这些问题,提出应根据食品成分特点优化样品前处理、完善设备维护制度、加强检测人员的专业培训和严格控制实验室环境条件的对策,以供参考。

基于HPLC本地通信技术的电动自行车充电监控系统设计

近年电动自行车在充电过程中发生的消防安全事故逐年增多,为避免电动自行车在充电过程中电池发生火灾隐患,急需开发符合电动自行车使用环境的电池充电监控系统,通过对电池的端电压、温度和瞬态跌落检测等方法,综合辨别电池的健康程度,并通过HPLC本地通信技术,将采集的电池状态经过充电线路传输到充电机,充电机会监控并记录每台自行车电池实时安全状态,控制充电开关。同时将每辆自行车的电池状态形成电子标签上传后台主站和云平台,为电动自行车电池的健康安全建立档案并为实时充电安全提供高效的监控手段。

改进双谱自适应功率调节算法的HPLC信道监测

宽带电力线载波通信HPLC信道容易受到非高斯白噪声信号影响,导致信道监测结果不精准。为此,提出了改进双谱自适应功率调节算法的HPLC信道监测方法。分析HPLC信道信号传输特性,构建信号衰落传递函数。采用改进双谱自适应功率调节算法,输出调节累积量结果,通过自回归调节时间序列傅里叶变换,获取双谱处理信号。采用周期性/睡眠监测机制,根据HPLC信道分类函数,实现HPLC信道监测。由实验结果可知,该方法在正常通信环境下获取的信道电压信号波动与实际输出的时域波形一致,在异常通信环境下信道电压信号波动只在部分时间段存在最大为20 V的波动误差,其余时间段与实际时域波形一致。

HPLC-ICP/MS用于测定鸡蛋中5种硒形态含量研究

为准确测定鸡蛋中硒代胱氨酸(SeCys2)、甲基硒代半胱氨酸(MeSeCys)、硒代蛋氨酸(SeMet)、硒酸根(Se(Ⅵ))和亚硒酸根(Se(Ⅳ))5种硒形态含量,研究建立一种利用高效液相色谱和电感耦合等离子体质谱联用技术快速测定方法(HPLC-ICP/MS),该方法鸡蛋样品中硒经蛋白酶XIV酶解和碘乙酰胺溶液提取,在Tris-HCl溶液中50℃水浴振荡4 h,4℃、10 000 r/min离心10 min,上清液采用0.22μm滤膜过滤后采用基质匹配外标法定量。结果显示:鸡蛋中5种硒形态在0~1 000.0μg/L浓度范围内,建立的检测方法具有良好的线性相关性,相关系数(R^(2))≥0.999;该方法对可食性鸡蛋中的硒检出限为0.23~0.95μg/kg,定量限为0.80~3.00μg/kg;5种硒形态中4种在低、中、高3个添加水平下,加标回收率为76.7%~103.1%,批内、批间变异系数均≤10%。研究表明,建立的HPLC-ICP/MS具有较高的灵敏度和精确度,为鸡蛋中5种硒形态的测定提供了适合检测方法。

HPLC-RID法测定聚乙烯醇滴眼液中的甘油

(目的)建立HPLC-RID法检测聚乙烯醇滴眼液中甘油的含量,以考察辅料处方添加的准确性,确保药物安全。(方法)采用高效液相色谱法,选择示差检测器,并选择磺酸型聚苯乙烯与二乙烯苯共聚体阳离子交换树脂H型为填充剂的色谱柱,建立甘油的含量测定方法,进行方法学验证后对聚乙烯醇滴眼液83批样品进行检测。(结果)聚乙烯醇滴眼液中甘油的质量分数为处方量的98.0%~103.3%。(结论)该方法专属性强、灵敏度高,适合于聚乙烯醇滴眼液中甘油的含量测定;甘油在制剂生产和贮存过程中含量稳定,企业对聚乙烯醇滴眼液中甘油的质量控制较好。