Determination of Major Phytohormones in Fourteen Different Seaweeds Utilizing SPE–LC–MS/MS

2019 ◽  
Vol 58 (2) ◽  
pp. 98-108 ◽  
Author(s):  
Sibel Yalçın ◽  
Emine Şükran Okudan ◽  
Özge Karakaş ◽  
Ayşe Nur Önem
Keyword(s):  
Liquid Chromatography ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Tandem Mass ◽  
Mass Detection ◽  
Hydrophilic Lipophilic Balance ◽  
Relative Standard ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass

Abstract Analysis of plant growth regulators (PGRs) should be approached by considering their extremely low concentrations and serious interfering effects that result from the matrix of various plant tissues. In the current research, the separation and simultaneous determination of different classes of phytohormones in 14 seaweeds collected from Turkey seashores were achieved by using solid-phase extraction (SPE) followed by a rapid and sensitive liquid chromatography tandem mass detection method. OASIS HLB (Hydrophilic-Lipophilic Balance) cartridges were successfully used for SPE process to eliminate the matrix effect and enhance the PGRs including zeatin, benzyl amino purine, indole-3-acetic acid, abscisic acid and gibberellic acid within partially different polarities. Based on the optimized experimental conditions, the method presented excellent performance related to linearity (r, 0.9996–0.9999) within the ranges of 0.5–500 ng/mL, relative standard deviation values ((1.43–2.01) for intraday and (2.36–3.50) for interday)), the limit of detection (0.01–0.84 μg/L) and the limit of quantification (0.02–2.76 μg/L). The obtained results confirm that the SPE–liquid chromatography/tandem mass spectrometry method performed is highly effective and convenient for routine analyses of trace amounts of the tested phytohormones in seaweeds and any other plant samples as well.

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 Multi-Class Determination of 64 Illicit Compounds in Dietary Supplements Using Liquid Chromatography–Tandem Mass Spectrometry

Molecules ◽  
2020 ◽  
Vol 25 (19) ◽  
pp. 4399
Author(s):  
Dasom Shin ◽  
Hui-Seung Kang ◽  
Hyungsoo Kim ◽  
Guiim Moon
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Dietary Supplements ◽  
Limit Of Detection ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass

In this work, liquid chromatography–tandem mass spectrometry (LC-MS/MS) method was developed and validated for screening and confirmation of 64 illicit compounds in dietary supplements. The target compounds were illegally used pharmaceutical drugs, prohibited compounds, and not authorized ingredients for different therapeutics (sexual enhancement, weight loss, muscular strengthening, and relaxing products). The validation procedure was performed to evaluate selectivity, linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy, and precision according to the Association of Official Analytical Chemists guidelines. The linearity was >0.98 in the range of 0.5–200 µg L−1. The LOQs were in the range 1–10 µg kg−1 for all target compounds. The accuracy (expressed as recovery) was 78.5–114%. The precision (expressed as the relative standard deviation) was below 9.15%. The developed method was applied for the determination of illicit compounds in dietary supplements collected from websites. As a result, the total detection rate was 13.5% (27 samples detected in 200 samples). The concentrations of detected samples ranged from 0.51 to 226 mg g−1. The proposed methodology is suitable for monitoring the adulteration of illicit compounds in dietary supplements.

scholarly journals Multiresidue Determination of Quinolone and Fluoroquinolone Antibiotics in Fish and Shrimp by Liquid Chromatography/Tandem Mass Spectrometry

2007 ◽  
Vol 90 (2) ◽  
pp. 604-612 ◽  
Author(s):  
Guy Dufresne ◽  
Andre Fouquet ◽  
Don Forsyth ◽  
Sheryl A Tittlemier
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Solid Phase ◽  
Tandem Mass ◽  
Fluoroquinolone Antibiotics ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass ◽  
Multiresidue Determination

Abstract A multiresidue method was developed to measure low levels of 8 fluoroquinolones (norfloxacin, ofloxacin, danofloxacin, ciprofloxacin, desethylene ciprofloxacin, enrofloxacin, sarafloxacin, and difloxacin) and 4 quinolones (oxolinic acid, flumequine, nalidixic acid, and piromidic acid). Method detection limits range from 0.1 ng/g for quinolones to 0.4 ng/g for fluoroquinolones. Average recoveries range from 57 to 96%, depending on analyte and commodity; relative standard deviations are all less than 18%. The drugs are extracted from tissues using a mixture of ethanol and 1% acetic acid, diluted in aqueous HCl, and defatted by extraction with hexane. The compounds are further isolated using cation-exchange solid-phase extraction and measured using liquid chromatography with electrospray tandem mass spectrometry detection. The method has been evaluated and applied to the analysis of salmon, trout, and shrimp. Detectable residues were observed in 10 out of 73 samples, at concentrations ranging from 0.28 to 16 ng/g.

scholarly journals Identification and Quantification of Dimethylamylamine in Geranium by Liquid Chromatography Tandem Mass Spectrometry

2012 ◽  
Vol 7 ◽  
pp. ACI.S9969 ◽  
Author(s):  
J.S. Li ◽  
M. Chen ◽  
Z.C. Li
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Plant Sample ◽  
Tandem Mass ◽  
Esi Ms ◽  
Relative Standard ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass

A sensitive and reliable method of liquid chromatography–electrospray ionization/tandem mass spectrometry (LC-ESI/MS/MS) was developed and validated for determining 1,3-dimethylamylamine (1,3-DMAA) and 1,4-dimethylamylamine (1,4-DMAA) in geranium plants ( Pelargonium graveolens). The sample was extracted with 0.5 M HCl and purified by liquid-liquid partition with hexane. The parameters for reverse-phase (C18) LC and positive ESI/MS/MS were optimized. The matrix effect, specificity, linearity, precision, accuracy and reproducibility of the method were determined and evaluated. The method was linear over a range of 0.10-10.00 ng/mL examined, with R 2 of 0.99 for both 1,3-DMAA and 1,4-DMAA. The recoveries from spiked concentrations between 5.00-40.00 ng/g were 85.1%-104.9% for 1,3-DMAA, with relative standard deviation (RSD) of 2.9%-11.0%, and 82.9%-101.8% for 1,4-DMAA, with RSD of 3.2%–-11.7%. The instrument detection limit was 1-2 pg for both DMAAs. The quantification limit was estimated to be 1-2 ng/g for the plant sample. This method was successfully applied to the quantitative determination of 1,3- and 1,4-DMAA in both geranium plant and geranium oil.

scholarly journals Simultaneous Determination of 16 Sulfonamides in Honey by Liquid Chromatography/TandemMass Spectrometry

2005 ◽  
Vol 88 (5) ◽  
pp. 1304-1311 ◽  
Author(s):  
Guo-Fang Pang ◽  
Yan-Zhong Cao ◽  
Jin-Jie Zhang ◽  
Guang-Qun Jia ◽  
Chun-Lin Fan ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Solid Phase ◽  
Phosphoric Acid Solution ◽  
Tandem Mass ◽  
Phase Extraction ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass ◽  
Oasis Hlb

Abstract A method is described for the determination of 16 sulfonamides in honey. Samples are dissolved in phosphoric acid solution (pH2), cleaned up with 2 solid-phase extraction (SPE) cartridges, an aromatic sulfonic cation-exchange cartridge and an Oasis HLB SPE cartridge, and analyzed both qualitatively and quantitatively by liquid chromatography/tandem mass spectrometry (LC/MS/MS) under the selected conditions. Without exception, calibration curves were linear (r = >0.995), when sulfamethizole was between 1.0 and 25.0 μg/kg; sulfacetamide, sulfapyridine, sulfadiazine, sulfachloropyridazine, sulfamethoxazole, sulfamerazine, sulfisoxazole, sulfamonomethoxine, and sulfadoxine were between 2.0 and 50.0 μg/kg; sulfamethoxypyridazine, sulfadimethoxine, and sulfathiazole were between 4.0 and 100.0 μg/kg; sulfamethazine and sulfameter were between 8.0 and 200.0 μg/kg; and sulfaphenazole was between 12.0 and 300.0 μg/kg. Average recoveries at 4 fortification levels in the range of 1.0–300 μg/kg in honey were 70.9–102.5%, and relative standard deviations were 2.02–11.52%. The limits of quantitation for the 16 sulfonamides were between 1.0 and 12.0 μg/kg, with the LC/MS/MS method.

scholarly journals Determination of Residues of 446 Pesticides in Fruits and Vegetables by Three-Cartridge Solid-Phase ExtractionGas Chromatography-Mass Spectrometry and Liquid Chromatography-Tandem Mass Spectrometry

2006 ◽  
Vol 89 (3) ◽  
pp. 740-771 ◽  
Author(s):  
Gao-Fang Pang ◽  
Chun-Lin Fan ◽  
Yong-Ming Liu ◽  
Yan-Zhong Cao ◽  
Jin-Jie Zhang ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Fruits And Vegetables ◽  
Solid Phase ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass ◽  
In Series

Abstract A method was developed for determination of residues of 446 pesticides in fruits and vegetables through the use of cleanup by a 3-cartridge solid-phase extractiongas chromatography/ mass spectrometry (GC/MS) and liquid chromatography/tandem mass spectrometry (LC/MS/MS). Fruit and vegetable samples (20 g) were extracted with 40 mL acetonitrile, salted out, and centrifuged. Half of the supernatant was passed into an Envi-18 cartridge, eluted with acetonitrile, and cleaned up with Envi-Carb and aminopropyl Sep-Pak cartridges in series after concentration of the eluates. Pesticides were eluted with acetonitriletoluene (3 + 1, v/v), and eluates were concentrated to 0.5 mL and then added into internal standards after solvent exchange with 2 mL hexane and used for determination of 383 pesticides by GC/MS. The other half of the supernatant was concentrated to 1 mL and cleaned up with Envi-Carb and aminopropyl Sep-Pak cartridges in series. Pesticides were eluted with acetonitriletoluene (3 + 1, v/v), and the eluates were concentrated to 0.5 mL, dried with nitrogen gas, diluted to 1.0 mL with acetonitrilewater (3 + 2, v/v), and used for determination of 63 pesticides by LC/MS/MS. The limit of detection for the method was 0.2600 ng/g depending on the individual pesticide. In the method, fortification recovery tests at high, medium, and low levels were conducted on 6 varieties of fruits and vegetables, i.e., apples, oranges, grapes, cabbage, tomatoes, and celery, with average recoveries falling within the range of 55.0-133.8% for 446 pesticides, among which average recoveries between 60.0-120.0% accounted for 99% of the results. The relative standard deviation was between 2.1-39.1%, of which a relative standard deviation of 2.1-25.0% made up 96% of the results. Experiments proved that the method was applicable for determination of residues of 446 pesticides in fruit and vegetables.

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