Determination of 222 pesticide residues in olive oil by fully automatic QuEChERS pre-treatment instrument coupled with gas chromatography-quadrupole-time-of-flight mass spectrometry DOI Open Access
Yan Liang,

Chunni Lei,

Bo Wang

и другие.

Chinese Journal of Chromatography, Год журнала: 2024, Номер 42(4), С. 368 - 379

Опубликована: Апрель 1, 2024

Pesticide residues may be present in olive oil because pesticides are applied to trees during their cultivation and growth for pest prevention some of these not easily degraded. Studies on pesticide have mainly focused the detection single types residues, reports simultaneous multiple limited. At present, hundreds with different polarities chemical properties used practice. id="p00010">In this study, an analytical method based fully automatic QuEChERS pretreatment instrument coupled gas chromatography-quadrupole time-of-flight mass spectrometry (GC-QTOF-MS) was established rapid determination 222 oil. The effects acetonitrile acidification concentration, n-hexane volume, oscillation time, centrifugation temperature, purification agent were investigated. First, ions good responses no obvious interference selected quantification characterization. process then developed by setting parameters optimal values. sample extracted containing 2% formic acid, supernatant purified a centrifuge tube 400 mg N-propylethylenediamine (PSA), octadecylsilane-bonded silica gel (C18), 1200 anhydrous magnesium sulfate. solution blown dry nitrogen fixed ethyl acetate instrumental analysis. Finally, matrix standard quantification. validated terms effects, linear ranges, limits (LODs) (LOQs), accuracies, precisions. results showed that 86.04% had ranges 0.02-2.00 μg/mL, 10.81% 0.10-2.00 3.15% 0.20-2.00 μg/mL. relationships within respective correlation coefficients (R2) greater than 0.99. LODs all tested ranged from 0.002 0.050 mg/kg, LOQs 0.007 0.167 mg/kg. Among determined, 170 mg/kg while 21 0.017 three spiked levels 0.2, 0.5, 0.8 79.58% average recoveries 70%-120% 65.92% 80%-110%. In addition, 93.54% relative deviations (RSDs, n=6)<10% 98.35% RSDs (n=6)<20%. 14 commercially available samples, seven detected range 0.0044-0.0490 fenbuconazole, chlorpyrifos, methoprene did exceed maximum stated GB 2763-2021. residual molinate, monolinuron, benalaxyl, thiobencarb been established. utilizes high resolution capability TOF-MS, which can improve throughput ensuring sensitivity. high-resolution accurate measurements render screening more reliable, is necessary high-throughput residues. use step reduces personnel errors labor costs, especially when large number samples must processed, thereby offering significant advantages over other approaches. Moreover, simple, rapid, sensitive, highly automatable, accurate, precise. Thus, it meets requirements provides reference development methods oils as well complex matrices.

Язык: Английский

Determination of 222 pesticide residues in olive oil by fully automatic QuEChERS pre-treatment instrument coupled with gas chromatography-quadrupole-time-of-flight mass spectrometry DOI Open Access
Yan Liang,

Chunni Lei,

Bo Wang

и другие.

Chinese Journal of Chromatography, Год журнала: 2024, Номер 42(4), С. 368 - 379

Опубликована: Апрель 1, 2024

Pesticide residues may be present in olive oil because pesticides are applied to trees during their cultivation and growth for pest prevention some of these not easily degraded. Studies on pesticide have mainly focused the detection single types residues, reports simultaneous multiple limited. At present, hundreds with different polarities chemical properties used practice. id="p00010">In this study, an analytical method based fully automatic QuEChERS pretreatment instrument coupled gas chromatography-quadrupole time-of-flight mass spectrometry (GC-QTOF-MS) was established rapid determination 222 oil. The effects acetonitrile acidification concentration, n-hexane volume, oscillation time, centrifugation temperature, purification agent were investigated. First, ions good responses no obvious interference selected quantification characterization. process then developed by setting parameters optimal values. sample extracted containing 2% formic acid, supernatant purified a centrifuge tube 400 mg N-propylethylenediamine (PSA), octadecylsilane-bonded silica gel (C18), 1200 anhydrous magnesium sulfate. solution blown dry nitrogen fixed ethyl acetate instrumental analysis. Finally, matrix standard quantification. validated terms effects, linear ranges, limits (LODs) (LOQs), accuracies, precisions. results showed that 86.04% had ranges 0.02-2.00 μg/mL, 10.81% 0.10-2.00 3.15% 0.20-2.00 μg/mL. relationships within respective correlation coefficients (R2) greater than 0.99. LODs all tested ranged from 0.002 0.050 mg/kg, LOQs 0.007 0.167 mg/kg. Among determined, 170 mg/kg while 21 0.017 three spiked levels 0.2, 0.5, 0.8 79.58% average recoveries 70%-120% 65.92% 80%-110%. In addition, 93.54% relative deviations (RSDs, n=6)<10% 98.35% RSDs (n=6)<20%. 14 commercially available samples, seven detected range 0.0044-0.0490 fenbuconazole, chlorpyrifos, methoprene did exceed maximum stated GB 2763-2021. residual molinate, monolinuron, benalaxyl, thiobencarb been established. utilizes high resolution capability TOF-MS, which can improve throughput ensuring sensitivity. high-resolution accurate measurements render screening more reliable, is necessary high-throughput residues. use step reduces personnel errors labor costs, especially when large number samples must processed, thereby offering significant advantages over other approaches. Moreover, simple, rapid, sensitive, highly automatable, accurate, precise. Thus, it meets requirements provides reference development methods oils as well complex matrices.

Язык: Английский

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