scholarly journals Determination of sweeteners in wine by liquid chromatography coupled with mass spectrometry (LC/MS)

2021 ◽  
Vol 36 (1) ◽  
pp. 32-44
Author(s):  
Nuno Neves ◽  
Natália Ribeiro ◽  
Cristina Esteves ◽  
Paulo Barros
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Limit Of Detection ◽  
Sweet Taste ◽  
Limit Of Quantification ◽  
Intermediate Precision ◽  
Wine Analysis ◽  
Minimal Sample ◽  
Wide Range ◽  
Sodium Cyclamate

Sweeteners are food additive substances that give a sweet taste to foods but their use in oenological practices is forbidden. Making use of the capabilities of liquid chromatography coupled with mass spectrometry, a method for wine analysis was developed and validated for the detection and quantitation of some of the most widely used sweeteners: aspartame, potassium acesulfame, sodium cyclamate, saccharin, sucralose and stevioside. A matrix-matched calibration was used for all compounds obtaining a linear concentration range from 50 μg/L to 1000 μg/L. The limit of detection ranged from 0.002 mg/L to 0.014 mg/L, and the limit of quantification varied between 0.005 mg/L and 0.048 mg/L. Precision and recovery were assessed for 50 μg/L, 250 μg/L and 1000 μg/L with repeatability and intermediate precision values from 0.6% to 21.6% and 2.7% to 26.4% respectively, and recoveries ranging from 60% to 126%. These results were achieved using minimal sample preparation with a fast and high throughput method that is applicable to a wide range of wine matrices.

scholarly journals Quantification of plasma remdesivir and its metabolite GS-441524 using liquid chromatography coupled to tandem mass spectrometry. Application to a Covid-19 treated patient

2020 ◽  
Vol 58 (9) ◽  
pp. 1461-1468 ◽  
Author(s):  
Jean-Claude Alvarez ◽  
Pierre Moine ◽  
Isabelle Etting ◽  
Djillali Annane ◽  
Islam Amine Larabi
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Half Life ◽  
Limit Of Detection ◽  
Treated Patient ◽  
Internal Standard ◽  
Therapeutic Drug ◽  
Active Metabolites ◽  
Limit Of Quantification ◽  
Positive Mode

AbstractObjectivesA method based on liquid chromatography coupled to triple quadrupole mass spectrometry detection using 50 µL of plasma was developed and fully validated for quantification of remdesivir and its active metabolites GS-441524.MethodsA simple protein precipitation was carried out using 75 µL of methanol containing the internal standard (IS) remdesivir-13C6 and 5 µL ZnSO4 1 M. After separation on Kinetex® 2.6 µm Polar C18 100A LC column (100 × 2.1 mm i.d.), both compounds were detected by a mass spectrometer with electrospray ionization in positive mode. The ion transitions used were m/z 603.3 → m/z 200.0 and m/z 229.0 for remdesivir, m/z 292.2 → m/z 173.1 and m/z 147.1 for GS-441524 and m/z 609.3 → m/z 206.0 for remdesivir-13C6.ResultsCalibration curves were linear in the 1–5000 μg/L range for remdesivir and 5–2500 for GS-441524, with limit of detection set at 0.5 and 2 μg/L and limit of quantification at 1 and 5 μg/L, respectively. Precisions evaluated at 2.5, 400 and 4000 μg/L for remdesivir and 12.5, 125, 2000 μg/L for GS-441524 were lower than 14.7% and accuracy was in the [89.6–110.2%] range. A slight matrix effect was observed, compensated by IS. Higher stability of remdesivir and metabolite was observed on NaF-plasma. After 200 mg IV single administration, remdesivir concentration decrease rapidly with a half-life less than 1 h while GS-441524 appeared rapidly and decreased slowly until H24 with a half-life around 12 h.ConclusionsThis method would be useful for therapeutic drug monitoring of these compounds in Covid-19 pandemic.

Occurrence of Naphthalene in Honey Consumed in Turkey as Determined by High-Pressure Liquid Chromatography

2007 ◽  
Vol 70 (7) ◽  
pp. 1735-1738 ◽  
Author(s):  
DİREN BEYOĞLU ◽  
GÜLDEN Z. OMURTAG
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Array Detector ◽  
Diode Array ◽  
Diode Array Detector ◽  
Signal To Noise ◽  
Limit Of Quantification ◽  
Naphthalene Concentration

This study is the first report on an investigation of the naphthalene concentration in samples of contaminated honey consumed in Turkey. Naphthalene was detected using high-performance liquid chromatography with a diode array detector at 220 nm. In one suspected contaminated specimen, the presence of naphthalene was confirmed by gas chromatography with mass spectrometry (GC-MS) at a concentration of 1.13 μg/kg. The limit of detection was 0.023 μg/g and the limit of quantification was 0.078 μg/g with signal-to-noise ratios of 3 and 10, respectively. A total of 100 samples of commercially available honey obtained from markets (53 samples) and street bazaars (47 samples) were analyzed. Mean naphthalene recovery from honey known to be contaminated with 1 μg/g was 80.4% (SD = 4.84%, n = 7).

scholarly journals Determination of Methomyl Residue in Tobacco Samples by Heart-Cutting Two-Dimensional Liquid Chromatography with Tandem Mass Spectrometry

2020 ◽  
Vol 2020 ◽  
pp. 1-6
Author(s):  
Shihao Shen ◽  
Min Chen ◽  
Tiannan Wang ◽  
Ting Fei ◽  
Dianhai Yang ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Dynamic Range ◽  
Limit Of Detection ◽  
High Sensitivity ◽  
Tandem Mass ◽  
Two Dimensional ◽  
Retention Performance ◽  
Limit Of Quantification

A novel heart-cutting two-dimensional liquid chromatography coupled with tandem mass spectrometry (2D-LC-MS/MS) was developed for the qualitative and quantitative analysis of methomyl residue in tobacco. Compared to traditional methodologies, fairly high sensitivity and stability were achieved, and the sample procedure was simplified in the two-dimensional liquid chromatography (2D-LC) method. Although methomyl had poor retention performance in most of the reversed-phase liquid chromatography (RPLC) columns, an effective RP/RP strategy was successfully facilitated. An XB-Phenyl column was employed in the first dimension to effectively remove thousands of interference compounds in the matrix. In the second dimension, an ADME column was applied for further separation. After optimization of the separation conditions, a six-way valve was utilized for direct transformation of the target fraction from the 1st column to the 2nd column. A dynamic range of 2.5 ng/mL to 500 ng/mL was achieved with correlation coefficient (r2) greater than 0.9995. The limit of detection and limit of quantification were determined to be 0.69 and 2.30 ng/mL, respectively. The 2D-LC method shows high sensitivity, good reproducibility, and recovery for methomyl in tobacco samples. Therefore, the new method was quite suitable for routine analysis.

scholarly journals Quantitative determination and validation of 17 cannabinoids in cannabis and hemp using liquid chromatography-tandem mass spectrometry

2020 ◽  
Vol 412 (27) ◽  
pp. 7381-7393 ◽  
Author(s):  
Garnet McRae ◽  
Jeremy E. Melanson
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Tandem Mass ◽  
Intermediate Precision ◽  
Chromatography Tandem Mass Spectrometry ◽  
Sample Extraction ◽  
Cannabidiolic Acid ◽  
Wide Range ◽  
Liquid Chromatography Tandem Mass

Abstract The increase in production of cannabis for medical and recreational purposes in recent years has led to a corresponding increase in laboratories performing cannabinoid analysis of cannabis and hemp. We have developed and validated a quantitative liquid chromatography-tandem mass spectrometry (LC-MS/MS) method that is simple, reliable, specific, and accurate for the analysis of 17 cannabinoids in cannabis and hemp. Liquid-solid sample extraction coupled with dilution into a calibration range from 10 to 10,000 ng/mL and LC-MS/MS analysis provides quantification of samples ranging from 0.002 to 200 mg/g (0.0002 to 20.0%) in matrix. Linearity of calibration curves in methanol was demonstrated with regression r2 ≥ 0.99. Within-batch precision (0.5 to 6.5%) and accuracy (91.4 to 108.0%) and between-batch precision (0.9 to 5.1%) and accuracy (91.5 to 107.5%) were demonstrated for quality control (QC) samples in methanol. Within-batch precision (0.2 to 3.6%) and accuracy (85.4 to 111.6%) and between-batch precision (1.4 to 6.1 %) and accuracy (90.2 to 110.3%) were also evaluated with a candidate cannabis certified reference material (CRM). Repeatability (1.5 to 12.4% RSD) and intermediate precision (2.2 to 12.8% RSD) were demonstrated via analysis of seven cannabis samples with HorRat values ranging from 0.3 to 3.1. The method provides enhanced detection limits coupled with a large quantitative range for 17 cannabinoids in plant material. It is suitable for a wide range of applications including routine analysis for delta-9-tetrahydrocannabinol (Δ9-THC), delta-9-tetrahydrocannabinolic acid (Δ9-THCA), cannabidiol (CBD), cannabidiolic acid (CBDA), and cannabinol (CBN) as well as more advanced interrogation of samples for both major and minor cannabinoids.

scholarly journals Determination of Polyphenol Components of Korean Prostrate Spurge (Euphorbia supina) by Using Liquid Chromatography—Tandem Mass Spectrometry: Overall Contribution to Antioxidant Activity

2014 ◽  
Vol 2014 ◽  
pp. 1-8 ◽  
Author(s):  
Yi Song ◽  
Sung Woo Jeong ◽  
Won Sup Lee ◽  
Semin Park ◽  
Yun-Hi Kim ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Limit Of Detection ◽  
Antioxidant Activities ◽  
Reducing Power ◽  
Tandem Mass ◽  
Limit Of Quantification ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

The Korean prostrate spurgeEuphorbia supinais a weed that has been used in folk medicine in Korea against a variety of diseases. Nine polyphenols were characterized for this plant by using high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) and the results were compared with the literature data. The individual components were validated using the calibration curves of structurally related external standards and quantified for the first time by using the validated method. Correlation coefficients (r2) were >0.9907. The limit of detection and limit of quantification of the method were >0.028 mg/L and 0.094 mg/L, respectively. Recoveries measured at 50 mg/L and 100 mg/L were 76.1–102.8% and 85.2–98.6%, respectively. The total amount of the identified polyphenols was 3352.9 ± 2.8 mg/kg fresh plant. Quercetin and kaempferol derivatives formed 84.8% of the total polyphenols. The antioxidant activities of the flavonoids were evaluated in terms of 1,1-diphenyl-2-picrylhydrazyl and 2,2′-azinobis(3-ethylbenzothiazoline-6-sulfonic acid) radical cation-scavenging activity, and the reducing power showed a dose-dependent increase. Cell viability was effectively suppressed at polyphenol mixture concentrations >250 mg/L.

Validation of a High-throughput Screening and Quantification Method for the Determination of Gabapentinoids in Blood Using a Combination of LC-TOF-MS and LC-MS-MS

2019 ◽  
Vol 43 (9) ◽  
pp. 696-702 ◽  
Author(s):  
Hilda De La Vega ◽  
Kim Fox ◽  
Justine Pardi ◽  
Wendy Santiago-Tirado ◽  
Gail Cooper
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
High Throughput ◽  
High Throughput Screening ◽  
Limit Of Detection ◽  
Blood Concentrations ◽  
Polysubstance Use ◽  
Wide Range ◽  
Blood Specimens ◽  
Tof Ms

Abstract Gabapentinoids such as gabapentin (GP) and pregabalin (PGL) have been used to treat a wide range of neurological and psychiatric disorders. In recent years, there has been an increasing awareness of GP and PGL misuse among individuals with a history of polysubstance use. Both GP and PGL are understood to potentiate the effects of opioids, with fatalities involving GP and PGL being reported with increasing frequency. An efficient procedure was developed to screen and quantitate GP and PGL in blood samples using a combination of liquid chromatography time-of-flight mass spectrometry (LC-TOF-MS) and liquid chromatography tandem mass spectrometry (LC-MS-MS). The developed LC-MS-MS method was linear from 0.5–50 mg/L, with a limit of detection (LOD) of 0.1 mg/L for GP and PGL. An LOD of 0.5 mg/L was determined for both analytes on the LC-TOF-MS screen. A total of 1,091 blood specimens were subjected to a protein crash with methanol, in the presence of deuterated internal standards, PGL-d6 and GP-d10, to minimize the effects of varying matrix conditions. Specimens tested included both post-mortem blood and preserved blood specimens collected for the purposes of investigating drug-impaired driving and suspected drug-facilitated crimes. Of the total of specimens tested, 101 (9.3%) screened positive using the developed LC-TOF-MS method for GP while only 13 (1.2%) blood specimens screened positive for PGL. All (100%) of the cases that screened positive for GP and PGL were confirmed positive by LC-MS-MS. Blood concentrations of GP and PGL ranged from <0.5 to 215 mg/L and from <0.5 to 32 mg/L, respectively. Of the blood specimens that had previously screened negative by LC-TOF-MS, 10% (N = 100) were randomly selected and tested by LC-MS-MS with 100% confirmed negative for GP and PGL. The developed methods provide a fast and reliable high-throughput screening and confirmation testing strategy for the detection of GP and PGL in blood specimens.

scholarly journals Application of an LC–MS/MS Method for the Simultaneous Quantification of Homovanillic Acid and Vanillylmandelic Acid for the Diagnosis and Follow-Up of Neuroblastoma in 357 Patients

Molecules ◽  
2021 ◽  
Vol 26 (11) ◽  
pp. 3470
Author(s):  
Narae Hwang ◽  
Eunbin Chong ◽  
Hyeonju Oh ◽  
Hee Won Cho ◽  
Ji Won Lee ◽  
...  
Keyword(s):  
Lower Limit ◽  
Large Scale ◽  
Homovanillic Acid ◽  
Limit Of Detection ◽  
Method Comparison ◽  
Vanillylmandelic Acid ◽  
Limit Of Quantification ◽  
Spot Urine ◽  
Minimal Sample ◽  
Clinical Biomarkers

Homovanillic acid (HVA) and vanillylmandelic acid (VMA) are end-stage metabolites of catecholamine and are clinical biomarkers for the diagnosis of neuroblastoma. For the first time in Korea, we implemented and validated a liquid chromatography tandem mass spectrometry (LC–MS/MS) assay to measure urinary concentrations of HVA and VMA according to Clinical and Laboratory Standards Institute guidelines. Our LC–MS/MS assay with minimal sample preparation was validated for linearity, lower limit of detection (LOD), lower limit of quantification (LLOQ), precision, accuracy, extraction recovery, carryover, matrix effect, and method comparison. A total of 1209 measurements was performed to measure HVA and VMA in spot urine between October 2019 and September 2020. The relationship between the two urinary markers, HVA and VMA, was analyzed and exhibited high agreement (89.1% agreement, kappa’s k = 0.6) and a strong correlation (Pearson’s r = 0.73). To our knowledge, this is the first study to utilize LC–MS/MS for simultaneous quantitation of spot urinary HVA and VMA and analyze the clinical application of both markers on a large scale for neuroblastoma patients.

Developments in mycotoxin analysis: an update for 2012-2013

2014 ◽  
Vol 7 (1) ◽  
pp. 3-33 ◽  
Author(s):  
F. Berthiller ◽  
P.A. Burdaspal ◽  
C. Crews ◽  
M.H. Iha ◽  
R. Krska ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Sample Preparation ◽  
Ergot Alkaloids ◽  
Tandem Mass ◽  
Wide Range ◽  
Rapid Spread ◽  
Food And Feed ◽  
Mycotoxin Analysis ◽  
The Individual

This review highlights developments in mycotoxin analysis and sampling over a period between mid-2012 and mid-2013. It covers the major mycotoxins: aflatoxins, Alternaria toxins, ergot alkaloids, fumonisins, ochratoxins, patulin, trichothecenes and zearalenone. A wide range of analytical methods for mycotoxin determination in food and feed were developed last year, in particular immunochemical methods and liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS)-based methods. After a section on sampling and sample preparation, due to the rapid spread and developments in the field of LC-MS/MS multimycotoxin methods, a separate section has been devoted to this area of research. It is followed by a section on mycotoxins in botanicals and spices, before continuing with the format of previous reviews in this series with dedicated sections on method developments for the individual mycotoxins.

High performance liquid chromatography (HPLC) method development and validation for the determination of flunixin: Animal plasma based study

2021 ◽  
pp. 1-11
Author(s):  
Sultan M. Alshahrani ◽  
John Mark Christensen
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Mobile Phases ◽  
Hplc Method Development ◽  
Development And Validation

This study was designed to develop and validate a simple and efficient high performance liquid chromatography (HPLC) method to determine flunixin concentrations in Asian elephant’s (Elephas maximus) plasma. Flunixin was administered orally at a dose of 0.8 mg/kg, and blood samples were collected. Flunixin extraction was performed by adding an equal amount of acetonitrile to plasma and centrifuging at 4500 rpm for 25 minutes. The supernatant was removed, and flunixin was analyzed using HPLC-UV detection. Two methods were developed and tested utilizing two different mobile phases either with or without adding methanol (ACN: H2O vs. ACN: H2O: MeOH). Both methods showed excellent linearity and reproducibility. The limit of detection was 0.05 ug/ml and limit of quantification was 0.1 ug/ml. the efficiency of flunixin recovery was maximized by the addition of methanol to mobile phase (ACN: H2O: MeOH as 50:30:20) at 95% in comparison to 23% without methanol. In conclusion, adding methanol to HPLC methods for extraction of flunixin from elephants’ plasma yielded higher recovery rate than without methanol.

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.

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