Determination of spinetoram in leafy vegetable crops using liquid chromatography and confirmation via tandem mass spectrometry

Abstract

Spinetoram is a second-generation member of the spinosyn class, all members of which have been shown to be effective in insect control via a novel mode of action. Spinetoram is a mixture of 3'-O-ethyl-5, 6-dihydro spinosyn J (XDE-175-J) and 3'-O-ethyl spinosyn L (XDE-175-L). In order to establish a determination method for the analysis of spinetoram residues in crops, commercial product (5% suspension concentrate spinetoram) was applied to two leafy vegetables (Garland chrysanthemum and Aster scaber) on different spraying schedules. The analytical method used herein was based on a reversed-phase separation on a C(18) column, isocratic elution and UV detection. The analytes were confirmed via tandem mass spectrometry. The method was linear over a concentration range of 0.05-10 ppm with a correlation coefficient in excess of 0.9998. The recoveries of XDE-175-J and XDE-175-L from the two vegetables ranged between 86.04 and 98.87% at spiking levels of 1 and 5 ppm. The relative standard deviations were no more than 7% for all recovery tests conducted herein. The calculated limits of detection and quantification were 0.01 and 0.03 ppm for both XDE-175-J and XDE-175-L. The levels of residues in two vegetables treated under a fixed schedule in the greenhouse were 6.21-0.55 ppm (maximum residue limit (MRL) = 7 ppm). In sum, this method constitutes an easy and reliable technique for the determination of spinetoram in leafy vegetables.

Residue and dissipation dynamic of spinetoram insecticide in pear fruits

“…Method for the determination of spinetoram residues in pear fruits validated completely fulfill the mentioned standard. HPLC-DAD was used for the analysis of spinetoram residues in tomato and leafy vegetables (Liu et al 2011;Malhat 2013;Hafez et al 2016), corresponding to the results obtained in this study.…”

Analytical approach, dissipation pattern and risk assessment of pesticide residue in green leafy vegetables: A comprehensive review

“…The complexity in sample treatment corresponds with the existing matrix interferences and the use of separation techniques, most commonly gas chromatography (Al Mahmud et al, ; D'Antuono et al, ; Farina et al, ; González‐Rodríguez, Rial‐Otero, Cancho‐Grande, & Simal‐Gándara, ; Ikeura, Kobayashi, & Tamaki, ; Park et al, ; Rahman, Sharma, et al, ; Srivastava, Trivedi, Srivastava, Lohani, & Srivastava, ; Tanaka et al, ; Van Dyk, Bouwman, Barnhoorn, & Bornman, ; Walorczyk, ) or liquid chromatography (Farha, Rahman, Abd El‐Aty, Jung, et al, ; Farha, Rahman, Abd El‐Aty, Kim, et al, ; S. W. Kim, Abd El‐Aty, et al, ; S. W. Kim, Rahman, et al, ; Lehotay & Cook, ; Liu et al, ; Pan, Xia, & Liang, ; Park et al, , ; Rahman et al, ; Wołejko et al, ).…”

“…All these factors led to complex matrices. To overcome the inference problems, liquid chromatography with ultraviolet absorbance detection (LC/UVD) is best (Farha, Rahman, Abd El‐Aty, Jung, et al, ; Farha, Rahman, Abd El‐Aty, Kim, et al, ; Liu et al, ), and to tackle suppression problems, the appropriate method might be LC associated with tandem mass spectrometry (LC–MS/MS) (S. W. Kim, Abd El‐Aty, et al, ; S. W. Kim, Rahman, et al, ; Na et al, ; Pan et al, ; Park et al, ; Rahman et al, ; Yang et al, ). Suppression problems increase the limits of quantification (LOQ) to equal to the MRL, which is expected to be 1/10.…”

Dynamic residual pattern of azoxystrobin in Swiss chard with contribution to safety evaluation

“…None of aforementioned methodologies considered the degradation dynamics as well as the PHRL. As LC‐UVD is the preferred technique for analysis (Farha, Abd El‐Aty, Rahman, Shin, & Shim, ; Farha et al, ; Liu et al, ) in modest laboratories having no tandem mass spectrometry. The present study planned to determine the residual levels of azoxystrobin in Swiss chard grown under greenhouse conditions using liquid–liquid extraction followed by HPLC‐UVD detection.…”