scholarly journals Multi Mycotoxins Analysis in Rice Using LC-MS/MS

2017 ◽  
Vol 1 (2) ◽  
pp. 77-84
Author(s):  
Riswahyuli Riswahyuli ◽  
Loise RS ◽  
Niza Nemara
Keyword(s):  
Solid Phase Extraction ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Extraction Column ◽  
Phase Extraction ◽  
Accurate Data ◽  
Develop Method ◽  
Limit Of Quantification ◽  
Novel Technology ◽  
Aflatoxin B2

Multi mycotoxins analysis in this research has the purpose to develop method of analysisfor rice sample with a simple and fast preparation and novel technology using LC-MS/MS. Several blankrice samples were spiked with standards of 8 classes of mycotoxins (Aflatoxin B1, Aflatoxin B2, AflatoxinG1, Aflatoxin G2, Deoxynivalenol, Zearalenon, T-2, and HT-2). Parameter of linearity, precision, recovery,limit of detection and limit of quantification were obtained and calculated. The result shows that all thevalidation parameters comply with criteria of method validation. Sonication method that was chosen toextract analites and Solid Phase Extraction Column that used for sample clean up are successful methodsthat have contribution for precise and accurate data. The Identification and quantification with LC-MS/MS help to determine and distinguish each mycotoxin through chromatogram appearance, retention timeand a specific m/z.

Development of a solid-phase extraction – spectrofluorimetric method for trace glutathione determination

2011 ◽  
Vol 89 (4) ◽  
pp. 517-523 ◽  
Author(s):  
Ke-Jing Huang ◽  
Cong-Hui Han ◽  
Ying-Ying Wu ◽  
Chao-Qun Han ◽  
De-Jun Niu ◽  
...  
Keyword(s):  
Solid Phase Extraction ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Signal To Noise Ratio ◽  
Calibration Graph ◽  
Extraction Column ◽  
Phase Extraction ◽  
Selective Reaction ◽  
Spectrofluorimetric Method ◽  
Relative Standard

A simple and efficient solid-phase extraction – spectrofluorimetric method has been developed to determine glutathione (GSH). Fluorescent probe N-(4,4-difluoro-5,7-dimethyl-4-bora-3a,4a-diaza-s-indacene-3-yl)methyl)iodoacetamide (BODIPY Fl-C1-IA) was used as the derivatization reagent. The procedure was based on a BODIPY Fl-C1-IA selective reaction with GSH to form the highly fluorescent product BODIPY Fl-C1-IA–GSH, using a solid-phase extraction column and spectrofluorimetric determination. The variables affecting analytical performance were studied and optimized. The calibration graph using the preconcentration system for GSH was linear over the range of 1–200 nmol/L with a limit of detection of 0.05 nmol/L (signal-to-noise ratio = 3). The relative standard deviation for six replicate determinations of GSH at the 100 nmol/L concentration level was 3.9%. The method was applied to water samples and average recoveries between 87.5% and 111.5% were obtained for spiked samples.

scholarly journals Greener Monolithic Solid Phase Extraction Biosorbent Based on Calcium Cross-Linked Starch Cryogel Composite Graphene Oxide Nanoparticles for Benzo(a)pyrene Analysis

Molecules ◽  
2021 ◽  
Vol 26 (20) ◽  
pp. 6163
Author(s):  
Aree Choodum ◽  
Nareumon Lamthornkit ◽  
Chanita Boonkanon ◽  
Tarawee Taweekarn ◽  
Kharittha Phatthanawiwat ◽  
...  
Keyword(s):  
Graphene Oxide ◽  
Solid Phase Extraction ◽  
Limit Of Detection ◽  
Solid Phase ◽  
High Sensitivity ◽  
Rice Flour ◽  
Oxide Nanoparticles ◽  
Phase Extraction ◽  
Limit Of Quantification ◽  
Significant Difference

Benzo(a)pyrene (BaP) has been recognized as a marker for the detection of carcinogenic polycyclic aromatic hydrocarbons. In this work, a novel monolithic solid-phase extraction (SPE) sorbent based on graphene oxide nanoparticles (GO) in starch-based cryogel composite (GO-Cry) was successfully prepared for BaP analysis. Rice flour and tapioca starch (gel precursors) were gelatinized in limewater (cross-linker) under alkaline conditions before addition of GO (filler) that can increase the ability to extract BaP up to 2.6-fold. BaP analysis had a linear range of 10 to 1000 µgL−1 with good linearity (R2 = 0.9971) and high sensitivity (4.1 ± 0.1 a.u./(µgL−1)). The limit of detection and limit of quantification were 4.21 ± 0.06 and 14.04 ± 0.19 µgL−1, respectively, with excellent precision (0.17 to 2.45%RSD). The accuracy in terms of recovery from spiked samples was in the range of 84 to 110% with no significant difference to a C18 cartridge. GO-Cry can be reproducibly prepared with 2.8%RSD from 4 lots and can be reused at least 10 times, which not only helps reduce the analysis costs (~0.41USD per analysis), but also reduces the resultant waste to the environment.

scholarly journals Presence of zearalenone in the most commonly grown wheat cultivars in Serbia

2013 ◽  
pp. 101-109 ◽  
Author(s):  
Igor Jajic ◽  
Sasa Krstovic ◽  
Biljana Perisic ◽  
Sandra Jaksic ◽  
Vojislava Bursic ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Solid Phase Extraction ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Phase Extraction ◽  
Wheat Cultivars ◽  
Limit Of Quantification ◽  
Average Value ◽  
Contamination Levels ◽  
Maximum Limit

A total of 45 samples of wheat from three different locations in Vojvodina were analyzed for the presence of zearalenone. Analytical methods based on clean-up by solid-phase extraction (SPE) columns and detection by liquid chromatography were used after validation. Limit of detection for ZEA in wheat was 18.6 ?g/kg and the limit of quantification was 56.5 ?g/kg. Recovery values ranged between 86% and 97%. The occurrence of ZEA in wheat was rather high with 53.3% of positive samples with the average value of 330 ?g/kg. Incidences were found from 68 ?g/kg to 1079 ?g/kg. Contamination levels were above the established maximum limit for unprocessed cereals, other than maize, in as many as seventeen samples. These results were compared to the results of investigation of deoxynivalenol and fumonisin content, established in our previous work on the same samples. The results obtained were also compared to those of the neighboring countries where the relevant data existed and to the data of previous studies in our country.

scholarly journals HPLC method validation and application for organic acid analysis in wine after solid-phase extraction

2016 ◽  
Vol 35 (2) ◽  
pp. 225 ◽  
Author(s):  
Violeta Ivanova-Petropulos ◽  
Krste Tašev ◽  
Marina Stefova
Keyword(s):  
Solid Phase Extraction ◽  
Organic Acids ◽  
High Performance ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Hplc Method ◽  
Phase Extraction ◽  
Hplc Separation ◽  
Limit Of Quantification

<p>A solid-phase extraction method followed by reverse phase high-performance liquid chromatography (RP-HPLC) was optimized and validated for the quantitative determination of tartaric, malic, shikimic, lactic, citric and succinic acids in wine. Solid-phase extraction was carried out with C18 cartridges and extraction recoveries for all acids ranging from 98.3 to 103% were obtained. HPLC separation was performed with isocratic elution on a LiChrosorb RP-18 column (250 × 4.6 mm I.D., 5 µm) protected with the appropriate guard column. The mobile phase was a 5 mM solution of H<sub>3</sub>PO<sub>4</sub> with pH 2.1 at a flow rate of 1 ml/min. Detection of the organic acids was performed at 210 nm. The developed method was validated by checking its linearity, limit of detection (LOD), limit of quantification (LOQ), precision and recovery. The method was applied to the analysis of organic acids in Macedonian red and white wines.</p>

scholarly journals Determination of Ranitidine in Human Plasma by SPE and ESI-LC-MS/MS for Use in Bioequivalence Studies

2013 ◽  
Vol 2013 ◽  
pp. 1-7
Author(s):  
Karini B. Bellorio ◽  
Maria Isabel R. Alves ◽  
Nelson R. Antoniosi Filho
Keyword(s):  
Solid Phase Extraction ◽  
Human Plasma ◽  
Extraction Method ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Internal Standard ◽  
Phase Extraction ◽  
Good Separation ◽  
Limit Of Quantification

A method for determining ranitidine in human plasma by ESI-LC-MS/MS was validated, using propranolol as internal standard. The extraction method used was solid phase extraction (SPE). Chromatographic separation was performed in a Chromolith C18 (50 mm × 4.6 mm i.d.) analytical column, which provided good separation of ranitidine and propranolol peaks with an analysis time of 2.5 minutes. Extraction yields of 94.4% for ranitidine and 89.4% for the internal standard were obtained. The lower limit of quantification (LLOQ) was 3.00 ng/mL, and limit of detection (LOD) was 0.05 ng/mL, with linearity ranging from 3.00 to 500 ng/mL. The results, thus, showed that this method is suitable for application in bioequivalence studies of ranitidine in human plasma.

scholarly journals METHOD OF THE RAPID ANALYSIS OF 20-HYDROXYECDYSONE CONTENT IN PLANTS AND FERNS USING SOLID-PHASE EXTRACTION ON POLYAMIDE AND MICROCOLUMN HPLC-UV

2018 ◽  
pp. 41-52
Author(s):  
Даниил (Daniil) Николаевич (Nikolaevich) Оленников (Olennikov) ◽  
Нина (Nina) Игоревна (Igorevna) Кащенко (Kashchenko)
Keyword(s):  
Solid Phase Extraction ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Reversed Phase ◽  
Flowering Plants ◽  
Pteridium Aquilinum ◽  
Phase Extraction ◽  
Limit Of Quantification ◽  
Preliminary Purification ◽  
Accuracy Indices

A method for the rapid quantitative analysis of 20-hydroxyecdysone in plants was developed using the microcolumn reversed-phase HPLC with UV detection (246 nm) on the  ProntoSIL-120-5-C18 column (2×75 mm) and the gradient eluent system LiClO4/HClO4-acetonitrile. The chromatographic stage of the analysis was 5 minutes long, which made it possible to characterize the technique as the fastest. For preliminary purification of the plant extracts, solid phase extraction on polyamide was used which led to an increase in the sensitivity of the analysis. Validation studies showed that the technique characterized by satisfactory metrological data. The values of the limit of detection (LOD) and the limit of quantification (LOQ) of 20-hydroxyecdysone were 3.3 and 10 μg/ml, respectively. The accuracy indices for various levels of 20-hydroxyecdysone content (80–120%) did not exceed 98.57–101.38%. The method applied to the analysis of 20-hydroxyecdysone in 359 species of flowering plants and 12 ferns species growing on the territory of the Buryatia Republic. The presence of 20-hydroxyecdysone was established in 22 species including 18 flowering plants and 4 ferns. The concentration levels of 20-hydroxyecdysone in plants varied from trace (Athyrium filix-femina, Diplazium sibiricum, Pteridium aquilinum) to very high (25.40 mg/g in Rhaponticum uniflorum and 25.87 mg/g in Silene jeniseensis). The presence of 20-hydroxyecdysone was firstly detected in three species including Gastrolychnis gracilis, G. saxatilis and Silene violascens. The developed technique is fast, simple, sensitive and stable and can be recommended for searching purpose to evaluate the new plant sources of 20-hydroxyecdysone.

scholarly journals Preparation and characterization of molecularly imprinted solid-phase extraction column coupled with high-performance liquid chromatography for selective determination of melamine

2018 ◽  
Vol 5 (9) ◽  
pp. 180750 ◽  
Author(s):  
Q. Zhou ◽  
X. C. Tan ◽  
X. J. Guo ◽  
Y. J. Huang ◽  
H. Y. Zhai
Keyword(s):  
Solid Phase Extraction ◽  
High Performance ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Cost Effective ◽  
Extraction Column ◽  
Phase Extraction ◽  
Molecularly Imprinted ◽  
Selective Determination ◽  
Solid Phase Extraction Column

We synthesized a selective molecularly imprinted solid-phase extraction (MIP-SPE) column and established an extraction and enrichment method using this MIP-SPE column. By coupling with HPLC, we developed a new method to detect trace amounts of melamine in eggs. The MIP-SPE column was synthesized by in situ thermal-initiated polymerization using melamine as the template, methacrylic acid as the functional monomer, ethylene glycol dimethacrylate as the cross-linker and azodiisobutyronitrile as the initiator. HPLC was used to evaluate the identification and enrichment capability of the MIP-SPE column and for the measurement of melamine in the sample. The melamine concentration exhibited an excellent linear relationship in the range of 0.1–25.0 µg ml −1 ( r = 0.9983). The identification capability of the MIP-SPE column was apparently superior to that of the non-imprinted polymer solid-phase extraction column; an average enrichment factor of 46.8-fold (RSD = 3.5%) was obtained for 0.4 µg ml −1 melamine by the MIP-SPE column. When the MIP-SPE HPLC method was applied to the detection of melamine in eggs, an average recovery rate of 93.5–102.0% (RSD = 3.6–4.9%) and a limit of detection of 0.05 µg kg −1 were obtained. This method is simple, fast and cost-effective; thus, it can greatly simplify the pre-treatment of complex samples and can be used in the detection of residual melamine in eggs and other products.

scholarly journals Solid Phase Extraction Method for the Determination of Atrazine and Cyanazine in Water Samples

2021 ◽  
Vol 14 ◽  
pp. 1-6
Author(s):  
Nurul Auni Zainal Abidin ◽  
Nur Sofiah Abu Kassim ◽  
Noor Hidayah Pungot
Keyword(s):  
Solid Phase Extraction ◽  
Water Samples ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Water System ◽  
Phase Extraction ◽  
Triazine Herbicides ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Spe Method

Triazine is one of the herbicides group that is widely used in agriculture that acts as an inhibitor for the growth of unwanted weeds in plants. The use of this herbicide on plants is absorbed by the soil and flows into a nearby water system. This research focused on two types of triazines, namely atrazine and cyanazine. This research aims to extract this type of triazine herbicides and to determine their concentration in water samples. It was quantified by using gas chromatography-electron capture detector (GC-ECD). Solid phase extraction (SPE) method was applied to extract herbicides from water samples. The results indicate that all the samples contained atrazine and cyanazine. Studies in the range of 0.5 - 25 mg/L achieved good linearity with good correlation of determination, r2 value of 0.9922 - 0.9982 mg/L. Relative standard deviations (RSD) for triplicate analysis of the samples were less than 10.0%. The limit of detection (LODs) and limit of quantification (LOQs) of cyanazine and atrazine were found, ranging from 3.33 – 6.67 μg/L and 11.09 – 20.10 μg/L, respectively. The recoveries of the triazine herbicides studied in water samples ranged from 82.5% to 107.6%. The developed method exhibited excellent clean-up capability and was successfully applied for determining triazine herbicide residues in water samples.

scholarly journals UPLC–TOF–MS Method for Simultaneous Quantification of Steroid Hormones in Tissue Homogenates of Zebrafish with Solid-Phase Extraction

Molecules ◽  
2021 ◽  
Vol 26 (20) ◽  
pp. 6213
Author(s):  
Yaxi Li ◽  
Zhi Yan ◽  
Xiaodong Li ◽  
Xiuli Yin ◽  
Ke Li
Keyword(s):  
Solid Phase Extraction ◽  
Steroid Hormones ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Whole Body ◽  
Tissue Homogenate ◽  
Spectrometric Analysis ◽  
Phase Extraction ◽  
Limit Of Quantification ◽  
Tof Ms

The quantification of steroid hormones of individual zebrafish (Danio rerio) provides perspective to understand endogenous hormone function. A UPLC–TOF–MS method was developed to provide a reproducible, sensitive, and efficient assay to determine the concentration of steroid hormones, including cortisol, testosterone, androstenedione, 11-deoxycortisol, 11-deoxycorticosterone, and 17-hydroxyprogesterone in whole-body homogenates of each zebrafish. Solid-phase extraction was used to sample matrix clean-up and acquired a recovery from 89.7% to 107.9%. The analytes were separated on an Aquity BEH C18 column using gradient elution. Mass spectrometric analysis was performed by single reaction monitoring (SRM) using positive electrospray ionization mode. The total running time was 6 min, which was greatly shortened compared with a previously reported method. The developed method exhibited excellent linearity for all the analytes, with regression coefficients higher than 0.99. The limit of detection varied between 0.1 and 0.5 ng/L and the limit of quantification was 0.5–1.7 ng/L for all analytes. The precision of the method was assessed on replicate measurements and was found to be in the ranges of 1.9 % to 6.6% and 4.3% to 8.6%, for intra- and inter-day analysis, respectively. This method was validated according to FDA guidance and applied to determine steroid hormone levels in the tissue homogenate of zebrafish acutely treated with caffeine and ethanol.

scholarly journals An Efficient Solid-Phase Extraction-Based Liquid Chromatography Method to Simultaneously Determine Diastereomers α-Tocopherol, Other Tocols, and Retinol Isomers in Infant Formula

2021 ◽  
Vol 2021 ◽  
pp. 1-8
Author(s):  
Baifen Huang ◽  
Zengxuan Cai ◽  
Jingshun Zhang ◽  
Jiaojiao Xu
Keyword(s):  
Liquid Chromatography ◽  
Solid Phase Extraction ◽  
Infant Formula ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Reversed Phase ◽  
Extraction Column ◽  
Phase Extraction ◽  
Chromatography Method ◽  
Macroporous Silica

The separation and simultaneous quantitation of diastereomers of DL-α-tocopherol, eight tocol forms, and retinols (trans and cis) have been conducted by reversed-phase liquid chromatography followed by solid-phase extraction. A chiral silica stationary phase modified with polysaccharide derivative on the monodisperse macroporous silica gel (Unichiral OD-5H column, 150 mm × 4.6 mm, 5 μm, NanoMicro Technology Co., Ltd.) was employed for eluting each target compound. Instead of conventional solvent extract, a green and eco-friendly solid-phase extraction column, packing with nonpolar polystyrene divinylbenzene, was optimized in terms of capacity and solvent used in steps. Validation of the method was examined and confirmed to be satisfactory, with excellent linearity regression (r > 0.9999), acceptable accuracy (74.66%∼112.92%), and precision (0.20%∼10.52%) results. Limit of detection ranged from 0.05 mg·kg−1 (retinols) to 0.4 mg·kg−1 (tocols). The method was checked by infant formula reference material SRM 1849a as well, which illustrated good agreement of mass fraction with certified value and enriched the important isomer data.

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