scholarly journals A Simple Method for the Screening and Measurement of Phenols in Dendrobium chrysotoxum by a Miniature Mass Detector Using a Matrix Solid-Phase Dispersion Method

2019 ◽  
Vol 2019 ◽  
pp. 1-9 ◽  
Author(s):  
Hongcheng Liu ◽  
Duo Mu ◽  
Tao Lin ◽  
Qiwan Li
Keyword(s):  
Limit Of Detection ◽  
Solid Phase ◽  
Limit Of Quantification ◽  
Simple Method ◽  
Mass Detector ◽  
Full Scan ◽  
Standard Solution ◽  
New Compounds

The present study aims at building a miniature mass method for the simultaneous determination of 12 phenols including the subtypes of bibenzyl, phenanthrene, and fluorenone, which was used to evaluate the quality of Dendrobium chrysotoxum. Through the full scan mode, new compounds were elucidated. The new compounds were quantified by carrying out the analysis of the ratio of the standard solution areas to new compound areas versus analyte concentration. The limit of detection (LOD) and limit of quantification (LOQ) for phenols were 0.5 µg/mL–1 µg/mL and 1 µg/mL–2 µg/mL, respectively. Average recoveries of phenols were ranged from 83.2% to 97.5%. Reproducibility represented by the RSD percentage was from 2.3% to 8.7%. The average content of the four analytes, erianin, chrysotobibenzyl, confusarin, and moscatilin, were more than 200 mg/kg, and the content of bibenzyl compounds was found to be the highest in Dendrobium chrysotoxum. Among these bibenzyl compounds, erianin was determined as the typical chemical marker from Dendrobium chrysotoxum. The newly established UPLC with a miniature mass detector method was found to be an appropriate tool for the quality assessment of Dendrobium chrysotoxum.

scholarly journals Determination of 77 Multiclass Pesticides and Their Metabolitesin Capsicum and Tomato Using GC-MS/MS and LC-MS/MS

Molecules ◽  
2021 ◽  
Vol 26 (7) ◽  
pp. 1837
Author(s):  
Harischandra Naik Rathod ◽  
Bheemanna Mallappa ◽  
Pallavi Malenahalli Sidramappa ◽  
Chandra Sekhara Reddy Vennapusa ◽  
Pavankumar Kamin ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Solid Phase ◽  
Graphitized Carbon Black ◽  
Limit Of Quantification ◽  
Gas And Liquid Chromatography ◽  
Relative Standard ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Primary Secondary Amine

A quick, sensitive, and reproducible analytical method for the determination of 77 multiclass pesticides and their metabolites in Capsicum and tomato by gas and liquid chromatography tandem mass spectrometry was standardized and validated. The limit of detection of 0.19 to 10.91 and limit of quantification of 0.63 to 36.34 µg·kg−1 for Capsicum and 0.10 to 9.55 µg·kg−1 (LOD) and 0.35 to 33.43 µg·kg−1 (LOQ) for tomato. The method involves extraction of sample with acetonitrile, purification by dispersive solid phase extraction using primary secondary amine and graphitized carbon black. The recoveries of all pesticides were in the range of 75 to 110% with a relative standard deviation of less than 20%. Similarly, the method precision was evaluated interms of repeatability (RSDr) and reproducibility (RSDwR) by spiking of mixed pesticides standards at 100 µg·kg−1 recorded anRSD of less than 20%. The matrix effect was acceptable and no significant variation was observed in both the matrices except for few pesticides. The estimated measurement uncertainty found acceptable for all the pesticides. This method found suitable for analysis of vegetable samples drawn from market and farm gates.

scholarly journals Oxytetracycline Residues in Honey Analyzed by Liquid Chromatography with UV Detection

2013 ◽  
Vol 57 (1) ◽  
pp. 25-32 ◽  
Author(s):  
Anna Gajda ◽  
Andrzej Posyniak ◽  
Andrzej Bober ◽  
Tomasz Błądek ◽  
Jan Żmudzki
Keyword(s):  
Liquid Chromatography ◽  
Oxalic Acid ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Experimental Treatment ◽  
Uv Detection ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Liquid Chromatography Method

Summary A liquid chromatography method with UV detection for determination of oxytetracycline (OTC) in honey has been developed. The samples were extracted with the solution of oxalic acid. The clean-up procedure was performed by solid phase extraction (SPE) using polymeric Strata X and carboxylic acid cartridges. Chromatographic separation was carried out on the Luna C8 analytical column with mobile phase consisting of acetonitrile-0.02 M oxalic acid. The method has been successfully validated according to the requirements of the European Decision 2002/657/EC and this method is used in routine control of oxytetracycline in honey samples. The limit of detection (LOD) and limit of quantification (LOQ) of the presented method were 10 and 12.5 μg/kg, respectively. The developed method has also been verified in quantitative determination of oxytetracycline residues in honey after experimental treatment with this product in bee colonies.

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 Extraction and Determination of Vitamin K1 in Foods by Ultrasound-Assisted Extraction, SPE, and LC-MS/MS

Molecules ◽  
2020 ◽  
Vol 25 (4) ◽  
pp. 839 ◽  
Author(s):  
Yueqing Xu ◽  
Liangxiao Zhang ◽  
Ruinan Yang ◽  
Xu Yu ◽  
Li Yu ◽  
...  
Keyword(s):  
Formic Acid ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Extraction Temperature ◽  
Vitamin K1 ◽  
Ultrasound Assisted Extraction ◽  
Limit Of Quantification ◽  
Assisted Extraction ◽  
Ultrasound Assisted

Vitamin K1 is one of the important hydrophobic vitamins in fat-containing foods. Traditionally, lipase is employed in the determination of vitamin K1 to remove the lipids, which makes the detection complex, time-consuming, and insensitive. In this study, the determination of vitamin K1 in fat-containing foods was developed based on ultrasound-assisted extraction (UAE), solid-phase extraction (SPE) combined with liquid chromatography–tandem mass spectrometry (LC-MS/MS). The optimal conditions for extraction of vitamin K1 were material–liquid ratio of 1:70 (g/mL), extraction temperature of 50 °C, extraction power of 700 W, extraction time of 50 min, material-wash fluid ratio of 1:60 (g/mL), and 8 mL of hexane/anhydrous ether (97:3, v/v) as the elution solvent. Then, vitamin K1 was analyzed on a ZORBAX SB-C18 column (50 mm × 2.1 mm, 1.8 μm) by gradient elution with water (0.01% formic acid) and methanol (0.01 formic acid + 2.5 mmol/L ammonium formate) as the mobile phase. The limit of detection (LOD) and limit of quantification (LOQ) were 0.05 and 0.16 μg/kg, respectively. Calibration curve was linear over the range of 10–500 ng/mL (R2 > 0.9988). The recoveries at three spiked levels were between 80.9% and 119.1%. The validation and application indicated that the proposed method was simple and sensitive in determination of vitamin K1 in fat-containing foods.

scholarly journals New Method for Simultaneous Determination of Microcystins and Cylindrospermopsin in Vegetable Matrices by SPE-UPLC-MS/MS

Toxins ◽  
2018 ◽  
Vol 10 (10) ◽  
pp. 406 ◽  
Author(s):  
Leticia Díez-Quijada ◽  
Remedios Guzmán-Guillén ◽  
Ana Prieto Ortega ◽  
María Llana-Ruíz-Cabello ◽  
Alexandre Campos ◽  
...  
Keyword(s):  
Chemical Structure ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Simultaneous Detection ◽  
Ultra Performance Liquid Chromatography ◽  
Limit Of Quantification ◽  
Worldwide Distribution ◽  
Exposure Estimation ◽  
Liquid Chromatography Tandem Mass

Cyanotoxins are a large group of noxious metabolites with different chemical structure and mechanisms of action, with a worldwide distribution, producing effects in animals, humans, and crop plants. When cyanotoxin-contaminated waters are used for the irrigation of edible vegetables, humans can be in contact with these toxins through the food chain. In this work, a method for the simultaneous detection of Microcystin-LR (MC-LR), Microcystin-RR (MC-RR), Microcystin-YR (MC-YR), and Cylindrospermopsin (CYN) in lettuce has been optimized and validated, using a dual solid phase extraction (SPE) system for toxin extraction and ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) for analysis. Results showed linear ranges (5–50 ng g−1 f.w.), low values for limit of detection (LOD) (0.06–0.42 ng g−1 f.w.), and limit of quantification (LOQ) (0.16–0.91 ng g−1 f.w.), acceptable recoveries (41–93%), and %RSDIP values for the four toxins. The method proved to be robust for the three variables tested. Finally, it was successfully applied to detect these cyanotoxins in edible vegetables exposed to cyanobacterial extracts under laboratory conditions, and it could be useful for monitoring these toxins in edible vegetables for better exposure estimation in terms of risk assessment.

Screening method for the determination of tetracyclines and fluoroquinolones in animal drinking water by liquid chromatography with diode array detector

2015 ◽  
Vol 18 (2) ◽  
pp. 283-289 ◽  
Author(s):  
E. Patyra ◽  
E. Kowalczyk ◽  
A. Grelik ◽  
M. Przeniosło-Siwczyńska ◽  
K. Kwiatek
Keyword(s):  
Drinking Water ◽  
Liquid Chromatography ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Screening Method ◽  
Array Detector ◽  
Diode Array ◽  
Diode Array Detector ◽  
Limit Of Quantification

Abstract A liquid chromatography – diode array detector (HPLC-DAD) procedure has been developed for the determination of oxytetracycline (OTC), tetracycline (TC), chlorotetracycline (CTC), doxycycline (DC), enrofloxacin (ENR), ciprofloxacin (CIP), sarafloxacin (SAR) and flumequine (FLU) residues in animal drinking water. This method was applied to animal drinking water. Solid-phase extraction (SPE) clean-up on an Oasis HLB cartridge allowed an extract suitable for liquid chromatographic analysis to be obtained. Chromatographic separation was carried out on a C18 analytical column, using gradient elution with 0.1% trifluoroacetic acid – acetonitrile – methanol at 30°C. The flow-rate was 0.7 mL/min and the eluate was analysed at 330 nm. The whole procedure was evaluated according to the requirements of the Commission Decision 2002/657/EC, determining specificity, decision limit (CCα), detection capacity (CCβ), limit of detection (LOD), limit of quantification (LOQ), precision and accuracy during validation of the method. The recoveries of TCs and FQs from spiked samples at the levels of 10, 100 and 1000 μg/L were higher than 82%. The developed method based on HPLC-DAD has been applied for the determination of four tetracyclines and four fluoroquinolones in animal drinking water samples.

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.

Full Scan Confirmation of Tetrahydrophthalimide in Whole Milk Using Gas Chromatography/Ion Trap Mass Spectrometry

1994 ◽  
Vol 77 (6) ◽  
pp. 1574-1579 ◽  
Author(s):  
Tina M P Chichila ◽  
D Ronald Erney
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Ion Trap ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Ion Trap Mass Spectrometry ◽  
Mass Spectral ◽  
Whole Milk ◽  
Full Scan

Abstract The determination of tetrahydrophthalimide (THPI) in whole milk extracts by gas chromatography/ion trap mass spectrometry (GC/ITMS) in the full-scan, electron impact (El) mode is presented. THPI is first isolated from whole milk by a procedure including protein precipitation, liquid–liquid partitioning, and 2 solid-phase extraction (SPE) cleanup steps. GC/ITMS in the El mode is used for the determinative step. The average recovery of THPI at fortification levels ranging from 5 to 54 ppb was 85.6% (n = 16, coefficient of variation = 9.13%). Full-scan mass spectral confirmation of THPI in milk extracts was obtained at the 5 ppb fortification level. The limit of detection was estimated to be 0.5 ppb. Chemical ionization also was used for THPI determination in whole milk extracts. The simultaneous isolation and determination of captan and captofol in whole milk are also discussed.

scholarly journals An Immunoenzymatic Method for the Determination of Ochratoxin A in Biological Liquids (Colostrum and Cow’s Milk)

Toxins ◽  
2021 ◽  
Vol 13 (10) ◽  
pp. 673
Author(s):  
Magdalena Cuciureanu ◽  
Cristina Tuchiluș ◽  
Anca Vartolomei ◽  
Bogdan Ionel Tamba ◽  
Lorena Filip
Keyword(s):  
Detection Limit ◽  
Ochratoxin A ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Biological Fluids ◽  
Cow’S Milk ◽  
Limit Of Quantification ◽  
Cow's Milk ◽  
Low Concentrations

Ochratoxins are mycotoxins that have been extensively studied lately due to the multiple toxic effects such as nephrotoxicity, hepatotoxicity, and carcinogenicity. These toxins contaminate plant and animal foods and after ingestion they reach into body fluids. The method of competitive direct enzyme immunoassay, in the solid phase, was validated through the determination of specific parameters (performance, linearity, recovery percentage, limit of detection, limit of quantification). The validated method was used to determine ochratoxin A in colostrum and cow’s milk. The method applied for the determination of ochratoxin A was linear for the concentration range of 0.0–0.5 ng/mL, the value for the regression coefficient (r) was 0.9838. Ochratoxin A was present in 91.67% of the colostrum and in 93.33% of cow’s milk samples. The linearity of the method, demonstrated for very low concentrations of analyte, the detection limit as well as the limit of quantification recommend the method for the determinations of micro-pollutants from foods, including biological fluids.

scholarly journals Validation of an analytical method for determination of eight food dyes in beverage and fruit roll-ups by ion-pair HPLC-DAD

2020 ◽  
Vol 22 (3) ◽  
pp. 126-134
Author(s):  
Maryam Zahedi ◽  
Amir Shakerian ◽  
Ebrahim Rahimi ◽  
Reza Sharafati Chaleshtori
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Food Additives ◽  
Ion Pair ◽  
Array Detector ◽  
Synthetic Dyes ◽  
Limit Of Quantification ◽  
Food Dyes

Background and aims: Synthetic dyes are widely used as food additives to avoid the loss of original dye in processed foods and to make the foods more attractive to consumers. For simultaneous determination of 8 most commonly used synthetic colors in beverage and foodstuff, an efficient, selective, and sensitive method is suggested. Methods: To analyze food colors in different beverages and fruit roll-ups, a method using Ion-pair high-performance liquid chromatography with diode array detector was suggested and validated. The separation of dyes from beverage and foodstuff was done by solid-phase extraction (SPE). The ultrasound-assisted solvent extraction method was used to extract dye from fruit roll-ups. Results: The limit of detection and the limit of quantification ranged from 0.036 to 0.07 and 0.098 to 0.2 µg/mL, respectively. IP-HPLC-DAD method was validated using precision (RSD %) and accuracy (Recovery %) of two concentrations of 0.5 and 1 µg/mL in terms of intra- and inter-day. SPE method was also validated using intra- and inter-day precision and accuracy. The most commonly detected dye in the tested samples was carmoisine with a concentration of 386 µg/g. Additionally, the concentration of dye was higher than the permitted level in 28.6% of beverages, 40% of edible ice products, and 100% of fruit roll-ups (Lavashak). Conclusion: This method is an effective, appropriate, accessible, reliable and safe analytic method to analyze eight food dyes

Sign in / Sign up

Export Citation Format

Share Document