Quantification of spinosyn A and spinosyn D in animal‐derived products using multiwalled carbon nanotubes coupled with LC–MS/MS for analysis

Abstract

An analytical method was developed for the quantification of spinosad (sum of spinosyns A and D) in five animal‐derived products (chicken breast, pork, beef, egg, and milk) using LC–MS/MS. The sample was extracted using acetonitrile/1% acetic acid and a combination of magnesium sulfate and sodium acetate salts. The sample was purified using multiwalled carbon nanotubes as sorbent via a dispersive‐solid‐phase extraction procedure. Matrix‐matched calibration (seven‐point) provided good linearity with coefficient of determination (R2) ≥0.99 for each product. The limits of detection and quantification (LOQs) ranged between 0.0003–0.03 and 0.001–0.1 mg/kg, respectively. Method validation was carried out after spiking the target standard to blank matrices at the concentration levels of LOQ, 2 × LOQ, and 10 × LOQ with three replicates for each. The average recoveries were between 74 and 104%, with relative standard deviations ≤9.68, which were within the acceptable range designated by the international organizations. The developed method was successfully applied for monitoring market samples collected throughout the Korean Peninsula, and none of the samples tested positive for the target analytes. It has therefore been shown that dehydration and acidification were effective to extract spinosad from animal‐derived products.

Simultaneous Analysis of Fenpropimorph and Fenpropimorph Acid in Six Different Livestock Products Using a Single-Sample Preparation Method Followed by Liquid Chromatography–Tandem Mass Spectrometry

“…Recovery tests were performed using milk and egg samples spiked to 5 µg kg −1 (limit of quantitation (LOQ), 10 µg kg −1 (2 × LOQ), and 50 µg kg −1 (10 × LOQ)). We used milk and egg typically to optimize sample preparation in the recovery tests, because they may have complex matrices that interfere with pesticide extraction, as reported previously [ 30 ]. We considered that if the recoveries from milk and egg met the SANTE criteria, those from the other four matrices would also be reproducible and reliable.…”

A Facile and Rapid Strategy for Quantifying PCBs in Cereals Based on Dispersive Solid-Phase Extraction and Gas Chromatography–Mass Spectrometry: A Reference for Safety Concerns in Sustainable Textiles

“…Multi-walled carbon nanotubes (MWCNTs) have a hollow multi-layered structure, abundant π electrons, and a large surface area [ 44 ]. They exhibit a good adsorption ability and are widely employed as dispersive SPE sorbents during food safety analyses of pesticides, veterinary drugs, and metals [ 45 , 46 , 47 , 48 , 49 ]. When functionalized with chemical groups (e.g., carboxyl, hydroxyl, and amine groups), they can gain better characteristics such as a larger surface area, better dispersion, and a greater negative charge on the surface than MWCNTs due to the functional groups [ 50 ].…”