Determination of Multiresidues of Three Acid Herbicides in Tobacco by Liquid Chromatography/Tandem Mass Spectrometry

Liu, Shanshan; Bian, Zhaoyang; Yang, Fei; Li, Zhonghao; Fan, Ziyan; Zhang, Hongfei; Wang, Ying; Zhang, Yange; Tang, Gangling

doi:10.5740/jaoacint.14-089

Cited by 5 publications

(8 citation statements)

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“…The method relies on SIM mode to establish sensitivity, shows LOQs of 0.1 and 5 ng mL −1 , and LODs of 0.1 and 1 ng mL −1 , for dicamba in water and air, respectively, and has acceptable reproducibility and repeatability. Detection limits reported by our evaluated method are within the range of previously reported LODs, which are 0.003–5 ng mL −1 using tandem MS [ 12 , 13 , 26 , 30 , 40 ]. The selection of a combination of precursor and fragment ions in SIM mode was found to improve detection sensitivity, and provides additional positive identification of dicamba.…”

Section: Discussionsupporting

confidence: 74%

“…Sub-picogram level detection of dicamba from water was also reported using paired-ion electrospray ionization (ESI) mass spectrometry [ 14 ]. Furthermore, several MS-based dicamba analytical methods have been reported for food items [ 17 , 18 ], water and agricultural cleanouts [ 13 , 14 , 16 , 19 , 20 , 21 , 22 ], air samplers [ 6 , 23 , 24 ], crops like apple, pepper, brown rice, and soybean [ 25 ], tobacco [ 26 ], barley [ 27 ], soybean [ 28 ], rice [ 29 ], as well as in other agricultural commodities [ 30 ]. Most of these protocols rely on triple quadrupole and/or higher resolution MS instruments, although quantification procedures using LC–diode array detection (DAD) [ 24 ] and single-quadrupole LC–MS [ 6 , 31 ] have been reported.…”

Section: Introductionmentioning

confidence: 99%

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Evaluation of a Stable Isotope-Based Direct Quantification Method for Dicamba Analysis from Air and Water Using Single-Quadrupole LC–MS

et al. 2020

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Dicamba is a moderately volatile herbicide used for post-emergent control of broadleaf weeds in corn, soybean, and a number of other crops. With increased use of dicamba due to the release of dicamba-resistant cotton and soybean varieties, growing controversy over the effects of spray drift and volatilization on non-target crops has increased the need for quantifying dicamba collected from water and air sampling. Therefore, this study was designed to evaluate stable isotope-based direct quantification of dicamba from air and water samples using single-quadrupole liquid chromatography–mass spectrometry (LC–MS). The sample preparation protocols developed in this study utilize a simple solid-phase extraction (SPE) protocol for water samples and a single-step concentration protocol for air samples. The LC–MS detection method achieves sensitive detection of dicamba based on selected ion monitoring (SIM) of precursor and fragment ions and relies on the use of an isotopically labeled internal standard (IS) (D3-dicamba), which allows for calculating recoveries and quantification using a relative response factor (RRF). Analyte recoveries of 106–128% from water and 88–124% from air were attained, with limits of detection (LODs) of 0.1 ng mL−1 and 1 ng mL−1, respectively. The LC–MS detection method does not require sample pretreatment such as ion-pairing or derivatization to achieve sensitivity. Moreover, this study reveals matrix effects associated with sorbent resin used in air sample collection and demonstrates how the use of an isotopically labeled IS with RRF-based analysis can account for ion suppression. The LC–MS method is easily transferrable and offers a robust alternative to methods relying on more expensive tandem LC–MS/MS-based options.

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Section: Discussionsupporting

confidence: 74%

Section: Introductionmentioning

confidence: 99%

Evaluation of a Stable Isotope-Based Direct Quantification Method for Dicamba Analysis from Air and Water Using Single-Quadrupole LC–MS

et al. 2020

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“…Nine sulfonylurea herbicides and one quinolinecarboxylic acid herbicide showed low recoveries in the 3.0-69.2% range with Cleanups 1-4 using GCB and/or PSA. The original QuEChERS method, employing PSA as the sorbent, showed weak recoveries (<70%) for sulfonylurea herbicides (Kaczyński & Łozowicka, 2017), which was ascribed to the known ability of PSA and GCB to absorb some weakly acidic herbicides such as sulfonylureas (Kaczyński & Łozowicka, 2017;Liu et al, 2015). A modified QuEChERS method employing C 18 cleanup was introduced by Lee et al (2016) to overcome this issue; consistent with their results, the best recoveries for sulfonylurea herbicides in strawberries were observed for Cleanup 5 with C 18 (Table 1).…”

Section: Cleanup Proceduresmentioning

confidence: 60%

“…A modified QuEChERS method employing C 18 cleanup was introduced by Lee et al (2016) to overcome this issue; consistent with their results, the best recoveries for sulfonylurea herbicides in strawberries were observed for Cleanup 5 with C 18 (Table 1). This outcome was rationalized by the fact that the C 18 sorbent has a lower affinity for acidic herbicides than PSA or GCB and features excellent performance during extract purification (Liu et al, 2015). The combination of C 18 and PSA (Cleanup 2) resulted in slightly higher recoveries of sulfonylurea herbicides, which, however, remained below 70%.…”

Section: Cleanup Proceduresmentioning

confidence: 99%

Multi-residue analysis of 203 pesticides in strawberries by liquid chromatography tandem mass spectrometry in combination with the QuEChERS method

Song

Yoo

Nam

2019

CyTA - Journal of Food

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Herein, a QuEChERS (quick, easy, cheap, effective, rugged, and safe) procedure together with liquid chromatography and tandem mass spectrometry was applied to the multi-residue analysis of 203 pesticides in strawberries. To reduce the amount of co-eluents, we compared several dispersive solidphase extraction cleanup procedures and found that cleanup using octadecylsilane provided the best recoveries. Spiked-sample recoveries of 70-120% with relative standard deviations of <20% were obtained for all tested pesticides except for quinmerac. Matrix-matched calibration curves exhibited good linearities (R 2 > 0.99), and the limits of quantification (LOQs) were lower than the maximum residue limits recommended by the European Commission and Korea Food and Drug Administration. The developed method was applied to real samples, revealing that their pesticide contents exceeded the corresponding LOQs. The obtained results demonstrate that octadecylsilane-based dispersive solid-phase extraction is a rapid and high-throughput cleanup procedure for the multi-residue analysis of pesticides in strawberries. Análisis de residuos múltiples de 203 pesticidas detectados en fresas empleando cromatografía líquida de espectrometría de masas en tándem en combinación con el método QuEChERS RESUMEN El presente estudio aplicó un procedimiento QuEChERS [acrónimo en inglés de rápido, fácil, barato, efectivo, resistente y seguro] junto con cromatografía líquida y espectrometría de masas en tándem para analizar residuos múltiples de 203 pesticidas detectados en fresas. Con el propósito de reducir la cantidad de coeluyentes, se compararon varios procedimientos de limpieza de extracción en fase sólida dispersiva, constatándose que la limpieza con octadecilsilano proporcionó las mejores recuperaciones. Así, se obtuvieron recuperaciones de muestras con picos de 70-120% y desviaciones estándar relativas <20% para todos los pesticidas analizados, excepto quinmerac. Las curvas de calibración de matriz coincidente exhibieron buenas linealidades (R 2 > 0.99), mientras que los límites de cuantificación (LOQ) fueron inferiores a los límites máximos de residuos (LMR) recomendados por la Comisión Europea y la Administración de Alimentos y Medicamentos de Corea. El método desarrollado se aplicó a muestras reales, revelando que los contenidos de pesticidas de éstas excedían los LOQ correspondientes. Los resultados obtenidos demuestran que la extracción dispersiva en fase sólida basada en octadecilsilano es un procedimiento de limpieza rápido y de alto rendimiento para analizar residuos múltiples de pesticidas en fresas.

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“…PSA, GCB, and C 18 are the sorbents most commonly used to remove co-extracts from fruits and vegetables during cleanup [28,29,30]; however, the optimal cleanup sorbent depends on the characteristics of the pesticide components and may vary as a consequence. PSA and GCB can adsorb some weakly acidic herbicides, including sulfonylureas [31]. As summarized in Table 3, the recovery rates of most sulfonylurea herbicides using d-SPE with PSA (cleanup 1–4) were found to be less than 70%.…”

Section: Resultsmentioning

confidence: 99%

Dispersive Solid–Liquid Extraction Coupled with LC-MS/MS for the Determination of Sulfonylurea Herbicides in Strawberries

Song

Seo

Choi

et al. 2019

Foods

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The monitoring of food quality and safety requires a suitable analytical method with simultaneous detection in order to control pesticide and herbicide residues. In this study, a novel analytical method, referred to as “dispersive solid–liquid extraction”, was applied to monitor seven sulfonylurea herbicides in strawberries. This method was optimized in terms of the amount of C18 and the volume of added water, and it was validated through satisfactory linearities (R2 > 0.99), recoveries of 70% to 84% with acceptable precisions, and limits of quantification lower than the maximum residue limits for the seven sulfonylurea herbicides in strawberries. The cleanup efficiency of the dispersive solid–liquid extraction technique was compared to that of the QuEChERS- (“quick, easy, cheap, effective, rugged and safe”) based method with dispersive solid phase extraction. The recoveries of the former were found to be comparable to those involving QuEChERS C18 cleanup (recoveries of 74%–87%). The method was used to determine sulfonylurea herbicide residues in ten strawberry samples. None of the samples had herbicide residues higher than that of limit of quantifications (LOQs) or maximum residue limits (MRLs). The results suggest that the dispersive solid–liquid extraction method combined with liquid chromatography-tandem mass spectrometry (LC-MS/MS) is effective for the analysis of sulfonylurea herbicide residues in strawberries.

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Determination of Multiresidues of Three Acid Herbicides in Tobacco by Liquid Chromatography/Tandem Mass Spectrometry

Cited by 5 publications

References 0 publications

Evaluation of a Stable Isotope-Based Direct Quantification Method for Dicamba Analysis from Air and Water Using Single-Quadrupole LC–MS

Evaluation of a Stable Isotope-Based Direct Quantification Method for Dicamba Analysis from Air and Water Using Single-Quadrupole LC–MS

Multi-residue analysis of 203 pesticides in strawberries by liquid chromatography tandem mass spectrometry in combination with the QuEChERS method

Dispersive Solid–Liquid Extraction Coupled with LC-MS/MS for the Determination of Sulfonylurea Herbicides in Strawberries

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