Rapid and Sensitive Detection of Aflatoxin B1, B2, G1 and G2 in Vegetable Oils Using Bare Fe3O4 as Magnetic Sorbents Coupled with High-Performance Liquid Chromatography with Fluorescence Detection

2020 ◽  
Vol 58 (7) ◽  
pp. 678-685
Author(s):  
Hui-Xian Zhang ◽  
Ping Zhang ◽  
Xiao-Fang Fu ◽  
You-Xiang Zhou ◽  
Xi-Tian Peng
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Vegetable Oil ◽  
Vegetable Oils ◽  
Aflatoxin B1 ◽  
High Performance ◽  
Solid Phase ◽  
Simultaneous Detection ◽  
Fluorescence Detector ◽  
Relative Standard

Abstract This paper reports a simple, sensitive and reliable method for the simultaneous detection of aflatoxin B1, B2, G1 and G2 in vegetable oils. Aflatoxins were extracted by magnetic solid phase extraction followed by high-performance liquid chromatography, then postcolumn photochemical derivatization and finally detected by fluorescence detector. Vegetable oil samples were first diluted with hexane and then commercial bare Fe3O4 nanoparticles were directly employed as sorbents to extract aflatoxins from complex vegetable oil samples, which significantly simplified the procedure of sample preparation and largely improved the sample analysis throughput. The effects of various parameters such as the amount of sorbent, loading, washing and eluting conditions were carefully optimized to improve the extraction efficiencies of aflatoxins. Under the optimal conditions, the limits of detection of four aflatoxins ranged from 0.01 μg/kg to 0.16 μg/kg, and squared regression coefficients (R2) >0.9990 were obtained within the linear range of 0.1–20 μg/kg (except for aflatoxin G2 with 0.5–20 μg/kg). Furthermore, the recoveries spiked at four concentration levels in a blank vegetable oil sample were from 82.6 to 106.2%, with inter- and intraday relative standard deviations <9.8%, indicating good accuracy and precision of the proposed method.

Determination of the Malachite Green in Sediment by High Performance Liquid Chromatography with Fluorescence Detection

2013 ◽  
Vol 781-784 ◽  
pp. 942-946 ◽  
Author(s):  
Jian Chao Deng ◽  
Xian Qing Yang ◽  
Lai Hao Li ◽  
Jian Wei Cen ◽  
Shu Xian Hao ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Malachite Green ◽  
Fluorescence Detection ◽  
High Performance ◽  
Solid Phase ◽  
Fluorescence Detector ◽  
Sediment Samples ◽  
Relative Standard

A new method of determination of malachite green (MG) in sediment has been developed by high performance liquid chromatography with fluorescence detection (HPLC-FLD). It is based on use of a deoxidation reaction which converts malachite green (MG) into LMG in the process of extraction. The sediment samples were extracted with a solution of formic acid and acetonitrile. Clean up and isolation was performed on MCX solid phase extraction (SPE) column. Chromatographic separation was achieved by using C18column with an isocratic mobile phase consisting of acetonitrile and ammonium acetate buffer (0.05 M, pH 4.5) (80:20, v/v). High performance liquid chromatography with fluorescence detector (λex=265 nm and λem=360 nm) was used for the determination of LMG. The recovery values of MG in sediment samples fortified with MG were determined by measuring the amount of MG in the samples, after carrying out deoxidation reaction with potassium borohydride, which converts the MG into LMG. Under the optimized conditions, the average recoveries of MG from sediment at three levels (1.0, 10 and 50 μg/kg) were 85.0% (range from 80.8 to 87.6%). Relative standard deviations (RSD) of recoveries at all fortification levels were less than for 9.57% for MG. The method detection limit obtained for MG was 0.5 μg/kg.

scholarly journals In Situ Synthesis of a Magnetic Graphene Platform for the Extraction of Benzimidazoles from Food Samples and Analysis by High-Performance Liquid Chromatography

2017 ◽  
Vol 2017 ◽  
pp. 1-11 ◽  
Author(s):  
Qianchun Zhang ◽  
Yulan Liu ◽  
Xingyi Wang ◽  
Huimin Li ◽  
Junyu Chen
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Solid Phase ◽  
Correlation Coefficients ◽  
Magnetic Solid Phase Extraction ◽  
Food Samples ◽  
Magnetic Graphene ◽  
Relative Standard

A novel method was proposed for the determination of five benzimidazoles (oxfendazole, mebendazole, flubendazole, albendazole, and fenbendazole) using magnetic graphene (G-Fe3O4). G-Fe3O4 was synthesized via in situ chemical coprecipitation. The properties of G-Fe3O4 were characterized by various instrumental methods. G-Fe3O4 exhibited a great adsorption ability and good stability towards analytes. Various experimental parameters that might affect the extraction efficiency such as the amount of G-Fe3O4, extraction solvent, extraction time, and desorption conditions were evaluated. Under the optimized conditions, a method based on G-Fe3O4 magnetic solid-phase extraction coupled with high-performance liquid chromatography was developed. A good linear response was observed in the concentration range of 0.100–100 μg/L for the five benzimidazoles, with correlation coefficients ranging from 0.9966 to 0.9998. The limits of detection (S/N=3) of the method were between 17.2 and 32.3 ng/L. Trace benzimidazoles in chicken, chicken blood, and chicken liver samples were determined and the concentrations of oxfendazole, mebendazole, flubendazole, and fenbendazole in these samples were 13.0–20.2, 1.62–4.64, 1.94–6.42, and 0.292–1.04 ng/g, respectively. The recovery ranged from 83.0% to 115%, and the relative standard deviations were less than 7.9%. The proposed method was sensitive, reliable, and convenient for the analysis of trace benzimidazoles in food samples.

scholarly journals Determination of Imazaquin Residues in Soil by Solid-Phase Extraction and High-Performance Liquid Chromatography

2007 ◽  
Vol 90 (2) ◽  
pp. 568-574 ◽  
Author(s):  
Chen Xuyan ◽  
Hu Jiye ◽  
Li Jianzhong
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Solid Phase Extraction ◽  
High Performance ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Phase Extraction ◽  
Application Rates ◽  
Relative Standard ◽  
Strong Anion Exchange

Abstract A method has been developed for the quantitation of imazaquin residues in soil. The herbicide was extracted from soil with methanolwater (2 + 1, v/v) and cleaned up by strong anion-exchange solid-phase extraction cartridges. Analysis was performed by using high-performance liquid chromatography with ultraviolet detection. Average recoveries through the method ranged from 90.7 to 100.6%, with relative standard deviation equal to or lower than 6.6%. The limit of detection was estimated to be 0.0015 mg/kg, and the minimum quantitation concentration of imazaquin in soil was 0.005 mg/kg. This method was successfully applied to evaluate imazaquin residue levels in soil and its dissipation rates in a soybean field in the Xisanqi District of Beijing, People's Republic of China. The dissipation study showed that the half life of imazaquin in soil was 10.37 0.0135 days at 3 different application rates.

scholarly journals Application of High Performance Liquid Chromatography to the Analysis of Pesticide Residues in Apple Juice

2018 ◽  
Vol 67 (1) ◽  
pp. 93-102 ◽  
Author(s):  
Lenche Velkoska-Markovska ◽  
Biljana Petanovska-Ilievska ◽  
Aleksandar Markovski
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Pesticide Residues ◽  
High Performance ◽  
Apple Juice ◽  
Solid Phase ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Standard Deviations

Summary The modern apple production involves the use of large amounts of pesticides that can be found in processed products such as apple juice. Harmful effects of pesticide residues on humans, especially children, are well known, hence the content of pesticide residues in fruit, vegetables and their juices should be controlled. This study presents an application of a new, relatively simple and reliable analytical method for qualitative and quantitative determination of three organophosphorus and one organonitrogen pesticide residues in apple juices. The analysis utilizes reversed-phase high-performance liquid chromatography (RP-HPLC) followed by UV diode array detection. Prior to HPLC analysis, a solid-phase extraction (SPE) was used for analytes concentration and sample clean-up. Specificity, selectivity, linearity, precision, accuracy and limit of quantification (LOQ) were examined to assess the validity of the developed method. The method had satisfactory values of multiple correlation coefficients for calibration curves (R2 ≥ 0.95 ). The precision was evaluated for the retention times and peak areas, and the estimated values for relative standard deviations (RSD) were 0.05 % - 0.18 % and 0.09 % - 0.62 %, respectively, which indicated an excellent precision of the proposed method. Under the established conditions, the recovery of analytes was 93.80 % - 119.41 %, with relative standard deviations below 0.56 %. This method was successfully applied for determination of some organophosphorus and organonitrogen pesticide residues in apple juices which were taken from Macedonian markets. The achieved values for LOQs were low enough compared to the MRLs of the investigated pesticides in apple according to the Regulation (EC) No 396/2005. Detectable residues of the examined pesticides were not found in the analyzed samples.

scholarly journals Monitoring Stevioside in Soju by High-Performance Liquid Chromatography and Liquid Chromatography/Mass Spectrometry

2007 ◽  
Vol 90 (5) ◽  
pp. 1365-1372 ◽  
Author(s):  
Fan Ni ◽  
Jeffrey Ammann ◽  
Abdul Mabud
Keyword(s):  
Mass Spectrometry ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Solid Phase ◽  
Single Step ◽  
Intermediate Precision ◽  
Relative Standard ◽  
Validation Parameters ◽  
Concentration Levels

Abstract A method using high-performance liquid chromatography (HPLC) with UV absorption detection was developed to monitor stevioside in soju, a distilled spirits product that is commercially available. The method uses a single-step dilution for sample preparation. It completely eliminates the time-consuming process of solid-phase extraction. A method using HPLC/mass spectrometry was optimized to confirm the identities of stevioside and other related impurities, including rebaudioside A, rebaudioside C, and dulcoside. The method was validated. The validation parameters included range (10.11007.3 ppm), precision, linearity, accuracy, robustness, system suitability, and intermediate precision. Stevioside standard solutions at 6 concentration levels were prepared for the validation work, including the tests for precision, linearity, and accuracy. The solutions were prepared in triplicate for each concentration. The relative standard deviation for the precision test was <3 for all 6 concentration levels. The correlation coefficient for the linearity within the concentration range was determined to be >0.999. The average recovery ranged from 95.7 to 101.1 for the soju samples spiked with stevioside standard. The detection limit for stevioside was estimated at 75 ppb. The method was used to screen several soju samples; no detectable stevioside was found in the samples.

scholarly journals Determination of Biotin by High-Performance Liquid Chromatography in Infant Formula, Medical Nutritional Products, and Vitamin Premixes

2006 ◽  
Vol 89 (6) ◽  
pp. 1515-1518 ◽  
Author(s):  
Linda B Thompson ◽  
Daniel J Schmitz ◽  
Shang-Jing Pan
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Infant Formula ◽  
High Performance ◽  
Solid Phase ◽  
Reversed Phase ◽  
Hplc Method ◽  
Fluorescence Detector ◽  
Sample Preparation Procedure

Abstract A solid-phase extraction sample preparation procedure was developed for use with a high-performance liquid chromatography (HPLC) method for biotin analysis. The HPLC method used a reversed-phase C18 column; chromatography run time was 8.5 min. After eluting from the column, biotin went through postcolumn reaction to form a conjugate with streptavidinfluorescein isothiocyanate, which was then detected by a fluorescence detector. This method was tested with infant formula, medical nutritional products, and vitamin premix samples.

scholarly journals SIMULTANEOUS METHOD FOR THE ESTIMATION OF BEDAQUILINE AND DELAMANID IN HUMAN PLASMA USING HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

2021 ◽  
pp. 36-40
Author(s):  
A. K. HEMANTH KUMAR ◽  
V. SUDHA ◽  
A. VIJAYAKUMAR ◽  
C. PADMAPRIYADARSINI
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Human Plasma ◽  
High Performance ◽  
Drug Exposure ◽  
Solid Phase ◽  
High Performance Liquid Chromatographic ◽  
Relative Standard ◽  
Validation Parameters ◽  
Mdr Tb

Objective: A specific, simple and sensitive high-performance liquid chromatographic method for the estimation of Bedaquiline (BDQ) and Delamanid (DLM) in human plasma was developed. Methods: The method involved deproteinization and further extracted the analyte using Solid Phase Extraction (SPE) cartridge and analysed using C18 column with the wavelength set at 231 nm. The isocratic mobile phase consisted of 10 mmol ammonium acetate buffer containing 0.25% acetic acid and 0.02% trifluoroacetic acid and acetonitrile in the ratio of 20:80(v/v). The validation parameters were evaluated. The method was applied to estimate plasma BDQ and DLM collected from five MDR-TB patients. Results: Well resolved peaks of BDQ and DLM at retention times of 5.4 and 2.6 min were obtained respectively. The calibration curve was linear over a range of 0.01–10.0 µg/ml for both BDQ and DLM. The intra-and inter-day relative standard deviations for standards were below 10%. The recoveries for BDQ ranged from 101% to 107% and 98% to 107 % for DLM respectively. Conclusion: A specific and sensitive method for simultaneous determination of BDQ and DLM in plasma using high-performance liquid chromatography was developed. This method can be used in clinical studies to evaluate drug exposure.

Ultrasound Assisted Dispersive Solid Phase Microextraction of Thymol and Carvacrol in Pharmaceutical Products Using Graphene Oxide as an Adsorbent Prior to Analysis by High Performance Liquid Chromatography

2020 ◽  
Vol 16 (5) ◽  
pp. 578-584
Author(s):  
Parvin Abedi Ghobadloo ◽  
Samin Hamidi ◽  
Mahboob Nemati ◽  
Fatemeh Soghra Jahed
Keyword(s):  
High Performance Liquid Chromatography ◽  
Graphene Oxide ◽  
Liquid Chromatography ◽  
Solid Phase Microextraction ◽  
High Performance ◽  
Solid Phase ◽  
Detection System ◽  
Ultra Violet ◽  
Pharmaceutical Products ◽  
Relative Standard

Background: Thymol and carvacrol are the most important dietary constituents in thyme species. These two active compounds are used for the standardization of pharmaceutical compounds. Objective: In this work, a simple and reliable ultrasonic assisted dispersive solid phase microextraction method (USA-DSPME) coupled with high performance liquid chromatography-ultra violet detection system was developed to determine thymol and carvacrol in pharmaceutical syrups. The efficiency of SPME sorbent was examined through several sorbents and finally Graphene Oxide (GO) was applied for extraction of the analytes. Method: The efficiency of GO was compared with three reduced forms of GO adsorbents as well. Several effective factors on the extraction performance were investigated. Results: Under the optimized conditions for the GO sorbent, inter and intra-day relative standard deviations (RSDs, n = 3) and the Limits of Detections (LODs) were lower than 5.0% and 0.02 μg/ml, respectively. Moreover, good linear ranges were observed in wide concentration ranges with R-squared larger than 0.9961 for both thymol and carvacrol. Conclusion: The present method is reliable and simple for determination of carvacrol and thymol in pharmaceutical products.

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