Simultaneous Determination of Nitroimidazoles and Quinolones in Honey by Modified QuEChERS and LC-MS/MS Analysis

This study reports an analytical method for the determination of nitroimidazole and quinolones in honey using liquid chromatography-tandem mass spectrometry (LC-MS/MS). A modified QuEChERS methodology was used to extract the analytes and determine veterinary drugs in honey by LC-MS/MS. The linear regression was excellent at the concentration levels of 1–100 ng/mL in the solution standard curve and the matrix standard curve. The recovery rates of nitroimidazole and quinolones were 4.4% to 59.1% and 9.8% to 46.2% with relative standard deviations (RSDs) below 5.2% and the recovery rates of nitroimidazole and quinolones by the matrix standard curve ranged from 82.0% to 117.8% and 79% to 115.9% with relative standard deviations (RSDs) lower than 6.3% in acacia and jujube honey. The acacia and jujube honeys have stronger matrix inhibition effect to nitroimidazole and quinolones residue; the matrix inhibition effect of jujube honey is stronger than acacia honey. The matrix standard curve can calibrate matrix effect effectively. In this study, the detection method of antibiotics in honey can be applied to the actual sample. The results demonstrated that the modified QuEChERS method combined with LC-MS/MS is a rapid, high, sensitive method for the analysis of nitroimidazoles and quinolones residues in honey.

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

Molecules ◽

10.3390/molecules26071837 ◽

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.

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Determination of Nine Microelements in Nostoc commune Vauch by ICP-AES

Advanced Materials Research ◽

10.4028/www.scientific.net/amr.518-523.5020 ◽

2012 ◽

Vol 518-523 ◽

pp. 5020-5023 ◽

Cited By ~ 1

Author(s):

Yi Diao ◽

Hong Bo Han ◽

Da Fen Zhang ◽

Jian Ping Zhou ◽

Zu Jun Yang

Keyword(s):

Toxic Elements ◽

Detection Limits ◽

Nostoc Commune ◽

Recovery Rates ◽

Relative Standard ◽

Standard Deviations

In this paper,the contents of nine elements including Cu, Fe, Mn, Zn, Al, Cd, Pb, Ti and V were determined by ICP-AES technique, which elements originated from Nostoc commune Vauch from different places. Detection limits ranged 0.0018 ug•ml-1 and 0.068 ug•ml-1, the relative standard deviations for all these elements were lower than 2%, and recovery rates ranged 95.8% and 105.6%. The results showed that there were rich elements in N. commune Vauch from different places; contens of Fe, Al and V were highest; contents of Mn, Zn and Ti were moderately high,and contents of Cu, Cd and Pb were lowest. Futhermore, Cu, Fe, Mn, Zn and V were essential to people’s health,and Al, Cd, Pb and Ti had potentially physiologically toxic.Finally,Concentrations of elements within N. commune Vauch from different places were different,which may have some relations with the soil and environment where N. Commune grew.As a result, the determining method which elements of N. Commune are determined by ICP-AES is rapid,accurate and convenient, and wild N. Commune may contain toxic elements because of pollutional soil and environment,so N. Commun cultivated artificially can effectively reduce harmful elements.

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

Analytical Chemistry Insights ◽

10.4137/aci.s9969 ◽

2012 ◽

Vol 7 ◽

pp. ACI.S9969 ◽

Cited By ~ 10

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.

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Determination of Residual Triflumezopyrim Insecticide in Agricultural Products through a Modified QuEChERS Method

Foods ◽

10.3390/foods10092090 ◽

2021 ◽

Vol 10 (9) ◽

pp. 2090

Author(s):

Sung-Min Cho ◽

Han-Sol Lee ◽

Ji-Su Park ◽

Su-Jung Lee ◽

Hye-Sun Shin ◽

...

Keyword(s):

Analytical Method ◽

Matrix Effects ◽

Solid Phase ◽

Reference Method ◽

Quechers Method ◽

Modified Quechers ◽

Relative Standard ◽

The Matrix ◽

Food Commodities

A rapid and simple analytical method for triflumezopyrim, a new class of mesoionic insecticides and commercialized molecules from DuPont, was developed with a modified QuEChERS method. The pH adjustment was used to improve the extraction efficiency of acetonitrile solvent, and dispersive solid-phase extraction was employed for the clean-up process. The five selected food commodities were used to verify the present optimized method, which displayed good linearity with an excellent correlation coefficient (R2 = 0.9992–0.9998) in the 0.003–0.30 mg/kg calibration range. The method limits of detection (LOD) and quantification (LOQ) were determined to be a value of 0.003 and 0.01 mg/kg, respectively. The mean recovery for the triflumezopyrim was in the 89.7–104.3% range. The relative standard deviations were ≤9.8% for intra- (n = 5) and inter-day (n = 15) precisions at concentrations of 0.01, 0.1, and 0.5 mg/kg in the five representative samples. The matrix effect has been calculated to confirm the effect during ionization of the analyte in the UPLC-MS/MS. The matrix effects of the instrumental analysis showed that triflumezopyrim was less susceptible to matrices. The proposed analytical method in this study has effectively improved the accuracy, selectivity, and sensitivity for the determination of triflumezopyrim in agricultural commodities; therefore, it can serve as a reference method for the establishment of maximum residue limits (MRLs).

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Determination of Microelements in Balanophora involucrate Hook. f. by ICP-AES

Applied Mechanics and Materials ◽

10.4028/www.scientific.net/amm.543-547.1132 ◽

2014 ◽

Vol 543-547 ◽

pp. 1132-1135

Author(s):

Hong Bo Han ◽

Yi Diao ◽

Hui Ping Wei ◽

Shu Quan Wan ◽

Da Fen Zhang

Keyword(s):

Toxic Elements ◽

Detection Limits ◽

Recovery Rates ◽

Relative Standard ◽

Standard Deviations

In this paper, the contents of these elements including Cu, Fe, Mn, Zn, Al, Cd, Pb, Ti and As were determined by ICP-AES technique, which elements originated from B. involucrate from different places. Detection limits ranged 0.0029 ug/ml-1 and 0.079 ug/ml-1, the relative standard deviations for all these elements were lower than 2%, and recovery rates ranged 94.8% and 105.8%. The results showed that there were rich elements in B. involucrate from different places; contents of Fe and Al were highest; contents of Mn, Zn, Cu and Ti were moderately high, and contents of As, Cd and Pb were lowest. Futhermore, Cu, Fe, Mn, Zn were essential to peoples health, and Al, Cd, As, Pb and Ti had potentially physiologically toxic. Finally, concentrations of elements within B. involucrate from different places were different, which may have some relations with the environment where B.involucrate grew. As a result, the determining method which elements of B. involucrate. are determined by ICP-AES is rapid, accurate and convenient, and wild B. involucrate may contain toxic elements because of pollutional soil and environment, so B.involucrate cultivated artificially can effectively reduce harmful elements.

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ICP-AES Determination of Elements in Elsholtzia rugulosa Hemsl. after Microwave Assisted Digestion

Applied Mechanics and Materials ◽

10.4028/www.scientific.net/amm.543-547.1136 ◽

2014 ◽

Vol 543-547 ◽

pp. 1136-1139

Author(s):

Hong Bo Han ◽

Yi Diao ◽

Hui Ping Wei ◽

Shu Quan Wan ◽

Da Fen Zhang

Keyword(s):

Detection Limits ◽

Recovery Rates ◽

Microwave Assisted ◽

Relative Standard ◽

Standard Deviations ◽

Microwave Assisted Digestion

In this paper, the contents of these elements including Cu, Fe, Mn, Zn, Al, Cd, Pb, Ti and As were determined by ICP-AES technique, which elements originated from E. rugulosa from different places. Detection limits ranged 0.0029 ug/ml-1 and 0.079 ug/ml-1, the relative standard deviations for all these elements were lower than 2%, and recovery rates ranged 93% and 105.8%. The results showed that there were rich elements in E. rugulosa from different places; contents of Fe and Al were highest; contents of Mn, Zn and Ti were moderately high; and contents of Cu, As, Cd and Pb were lowest. Finally, concentrations of elements within E. rugulosa from different places were different, which may have some relations with the environment where it grew. As a result, the determining method which elements of E. Rugulosa are determined by ICP-AES is rapid, accurate and convenient.

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Determination of Hexabromocyclododecanes in Fish Using Modified QuEChERS Method with Efficient Extract Clean-Up Prior to Liquid Chromatography–Tandem Mass Spectrometry

Separations ◽

10.3390/separations7030044 ◽

2020 ◽

Vol 7 (3) ◽

pp. 44

Author(s):

Linda Okšová ◽

Peter Tölgyessy

Keyword(s):

Mass Spectrometry ◽

Liquid Chromatography ◽

Tandem Mass Spectrometry ◽

Tandem Mass ◽

Quechers Method ◽

Modified Quechers ◽

Chromatography Tandem Mass Spectrometry ◽

Relative Standard ◽

Liquid Chromatography Tandem Mass

A modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) sample preparation method coupled with liquid chromatography–tandem mass spectrometry (LC–MS/MS) was proposed for the determination of α-, β-, and γ-hexabromocyclododecane (HBCD) diastereomers in whole-fish homogenate samples. The main modification of the QuEChERS method concerned a clean-up step in which the combination of pH-tuned dispersive liquid–liquid microextraction (DLLME) with 18.4 M H2SO4 digestion allowed to successfully eliminate the matrix substances from the final extract. For the target HBCDs, good response linearity was obtained with coefficients of determination (R2) >0.998 for the concentration range corresponding to 0.1–50 ng of analyte per g of sample. Limits of quantifications (LOQs) were 0.15–0.25 ng g−1 ww (wet weight), and the recoveries from samples spiked at levels of 0.5 and 5 ng g−1 ranged from 89% to 102% with relative standard deviations <7.5%. The accuracy of the method was verified by analysis of the NIST standard reference material SRM 1947, and a good agreement (90%) was obtained with the certified value for the α-HBCD present in the sample. Finally, the method was applied to the analysis of 293 fish samples collected in water bodies from all over Slovakia, in which the highest concentrations were determined for α-HBCD with the maximum value of 31 ng g−1 ww.

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

Journal of Chromatographic Science ◽

10.1093/chromsci/bmz074 ◽

2019 ◽

Vol 58 (2) ◽

pp. 98-108 ◽

Cited By ~ 2

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.

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