On‐line solid‐phase extraction for liquid chromatography–mass spectrometry analysis of pesticides

A novel fully automated method based on dual column switching using turbulent flow chromatography followed by liquid chromatography with tandem mass spectrometry was developed for the determination of aflatoxin B1 , B2 , G1 , and G2 in corn powder, edible oil, peanut butter, and soy sauce samples. After ultrasound-assisted extraction, samples were directly injected to the chromatographic system and the analytes were concentrated into the clean-up loading column. Through purge switching, the analytes were transferred to the analytical column for subsequent detection by mass spectrometry. Different types of TurboFlow(TM) columns, transfer flow rate, transfer time were optimized. The limits of detection and quantification of this method ranged between 0.2-2.0 and 0.5-4.0 μg/kg for aflatoxins in different matrixes, respectively. Recoveries of aflatoxins were in range of 83-108.1% for all samples, matrix effects were in range of 34.1-104.7%. The developed method has been successfully applied in the analysis of aflatoxin B1 , B2 , G1 , and G2 in real samples.

Section: Introductionmentioning

confidence: 99%

Simultaneous determination of aflatoxin B₁, B₂, G₁, and G₂ in corn powder, edible oil, peanut butter, and soy sauce by liquid chromatography with tandem mass spectrometry utilizing turbulent flow chromatography

Fan

Zhang

et al. 2015

“…Usually, if the plasma sample was injected directly into the SPE column, the proteins and other matrix in plasma would cover the surface of SPE particles so that the adsorption capacity of SPE column would decrease significantly . Therefore, the loading solvent that diluted the injected sample solution could greatly affect the extraction of SPE.…”

Section: Resultsmentioning

confidence: 99%

Automatic on‐line solid‐phase extraction with ultra‐high performance liquid chromatography and tandem mass spectrometry for the determination of ten antipsychotics in human plasma

Zhong

Shen

Liu

et al. 2016

An automatic on-line solid-phase extraction with ultra-high performance liquid chromatography and tandem mass spectrometry method was developed for the simultaneous determination of ten antipsychotics in human plasma. The plasma sample after filtration was injected directly into the system without any pretreatment. A Shim-pack MAYI-C8 (G) column was used as a solid-phase extraction column, and all the analytes were separated on a Shim-pack XR-ODS III column with a mobile phase consisting of 0.1% v/v formic acid in water with 5 mM ammonium acetate and acetonitrile. The method features were systematically investigated, including extraction conditions, desorption conditions, the equilibration solution, the valve switching time, and the dilution for column-head stacking. Under the optimized conditions, the whole analysis procedure took only 10 min. The limits of quantitation were in the range of 0.00321-2.75 μg/L and the recoveries ranged from 75.9 to 122%. Compared with the off-line ultra-high performance liquid chromatography and the reported methods, this validated on-line method showed significant advantages such as minimal pretreatment, shortest analysis time, and highest sensitivity. The results indicated that this automatic on-line method was rapid, sensitive, and reliable for the determination of antipsychotics in plasma and could be extended to other target analytes in biological samples.

“…LC in combination with MS/MS has become more popular for multiresidue analysis due to its high specificity and excellent separation for the target compounds, and it has been proven to be an excellent analytical tool for multiresidue detection of pollutants in different matrices [18][19][20]. In the current experiment, herbicides were analyzed by injection of individual standards at 500 g/L in MRM mode, and the three target compounds were ionized to comparable degrees in both positive and negative modes.…”

Section: Optimization Of Ms/ms Parametersmentioning

confidence: 99%

Simultaneous determination of three herbicides in wheat, wheat straw, and soil using a quick, easy, cheap, effective, rugged, and safe method with ultra high performance liquid chromatography and tandem mass spectrometry

Zhao

Dong

et al. 2015

In this study, a sensitive and effective analytical method for the extraction and detection of three herbicide residues (florasulam, fluroxypyr, and halauxifen-methyl) in wheat and soil was developed. Samples were extracted with acetonitrile/water followed by salting out, dispersive solid-phase extraction cleanup, and detection using ultra high performance liquid chromatography coupled with tandem mass spectrometry. The target analytes were detected within a 5 min runtime using an ultra high performance liquid chromatography high-strength silica trifunctional column connected to an electrospray ionization source in positive mode. The method was validated in five replicates at three fortification concentrations in each matrix. Adequate pesticide quantification and identity confirmation were attained, even at the lowest concentration levels. The method showed very good accuracy and precision. Good recoveries were observed for the three herbicides and mostly ranged between 75.8 and 114.6%, with intraday relative standard deviations <6.01% and interday relative standard deviations <4.02%. The limits of quantification ranged between 0.14 and 7.68 μg/kg for each herbicide. The method was successfully applied for the simultaneous analysis of the three herbicides in actual trial samples, and the results proved that the proposed method was effective in detecting these three herbicides.