A combination of solid‐phase extraction and dispersive solid‐phase extraction effectively reduces the matrix interference in liquid chromatography–ultraviolet detection during pyraclostrobin analysis in perilla leaves

Abstract

Perilla leaves contain many interfering substances; thus, it is difficult to protect the analytes during identification and integration. Furthermore, increasing the amount of sample to lower the detection limit worsens the situation. To overcome this problem, we established a new method using a combination of solid-phase extraction and dispersive solid-phase extraction to analyze pyraclostrobin in perilla leaves by liquid chromatography with ultraviolet absorbance detection. The target compound was quantitated by external calibration with a good determination coefficient (R(2) = 0.997). The method was validated (in triplicate) with three fortification levels, and 79.06- 89.10% of the target compound was recovered with a relative standard deviation <4. The limits of detection and quantification were 0.0033 and 0.01 mg/kg, respectively. The method was successfully applied to field samples collected from two different areas at Gwangju and Muan. The decline in the resiudue concentrations was best ascribed to a first-order kinetic model with half-lives of 5.7 and 4.6 days. The variation between the patterns was attributed to humidity.

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

“…Significant effort has been made to develop and test novel analytical tools and methodologies in pesticide science. If the experimental sample is not sufficiently large to represent the original lot or unit, the total cost, time and efficiency associated with using the advanced analytical instruments and methodologies will not provide useful conclusions, and may result in confusing data (Farha, Rahman, Abd El‐Aty, Jung, et al, ; Lehotay & Cook, ). Therefore, the Ministry of Food and Drug Safety, Republic of Korea () of the Republic of Korea endorsed a sample weight of 20–25 g for extraction to lessen sampling error, to ensure experimental sample homogeneity and to secure low detection limits and quantification with higher precision, thereby enabling MRL compliance.…”

“…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, ).…”

Residue behaviours, dissipation kinetics and dietary risk assessment of pyaclostrobin, cyazofamid and its metabolite in grape

“…Different methods have been developed for the determination of pyraclostrobin, for example, gas chromatography which requires cumbersome sample preparation and large amounts of organic solvents . Capillary electrophoresis and subsequent liquid chromatography (LC) UV and mass spectrometry (MS) have been utilized for the determination of pyraclostrobin in different matrices, such as apple, citrus, pepper, peanut, rice, grape . Besides, attention has been paid to the change of pyraclostrobin in food processing such as rasin and paste preparation.…”

Quick, easy, cheap, effective, rugged, and safe sample preparation approach for pesticide residue analysis using traditional detectors in chromatography: A review

“…Even after using c‐SPE (silica/ Florisil®) to purify 5 g of leafy vegetables (perilla leaves), the target analyte was not protected against interference in the UV detection. Additional d‐SPE cleanup has been employed to overcome this problem, which requires additional time and labor . In this case, the double‐layer c‐SPE concept proposed by Lehotay et al.…”