Combination of Modified QuEChERS and Disposable Polyethylene Pipet Assisted DLLME Based on Low Density Solvent Extraction for Rapid and Sensitive Determination of Fipronil and Its Metabolites in Eggs by GC-MS

Development, validation, and use of a monitoring method for fipronil and its metabolites in chicken eggs by QuEChERS with online‐SPE‐LC‐Q/Orbitrap analysis

“…To date, several methods have been proposed for the determination of fipronil and its metabolites in a variety of matrices, such as meat, 12 honey, 13,14 oil crops, 15 vegetables, 5,[16][17][18] fruits, 17,19 and eggs. 7,[20][21][22] Most analytical techniques are based on chromatographic techniques such as high-performance liquid chromatography (HPLC), 13,23 liquid chromatography tandem mass spectrometry (LC-MS/MS), 14,24,25 liquid chromatography-highresolution mass spectrometry (LC-HRMS), 26,27 gas chromatography (GC), 28,29 and gas chromatography tandem mass spectrometry (GC-MS or GC-MS/MS). 5,18,30 Among these detection techniques, Q Exactive Orbitrap HRMS is ideal for biological sample analysis due to its high mass resolution, high mass accuracy, and high-performance quadrupole for selectivity.…”

“…China promulgated in 2009). Nevertheless, the “Dutch poisonous egg” event raised by the inappropriate use of fipronil in Belgium in 2017 caused a sensational effect worldwide 7 . The concentration of fipronil in the eggs reached 1.2 mg kg −1 , which far exceeded the maximum residue level (MRL) set by the Codex Alimentarius Commission (CAC) (0.02 mg kg −1 ), 8 Japan (0.02 mg kg −1 ), 9 the United States (0.03 mg kg −1 ), 10 and many other countries for the sum of fipronil and its metabolites in eggs 11 .…”

“…In previous reports, liquid‐phase extraction (LPE) with acetonitrile (ACN) was mostly used for the extraction of fipronil and its metabolites from eggs. Afterwards, cleanup methods, such as solid‐phase extraction (SPE) 30,32 ; magnetic solid‐phase extraction, 33 dispersive SPE, 20 and quick, easy, cheap, effective, rugged, and safe (QuEChERS), 6,7,11 were adopted to remove the interferences of the matrix in eggs. The addition of extraction solvent dilutes the concentration of analytes, and the samples usually need to be enriched by evaporation and reconstitution in these traditional methods 21,30,32,34 .…”

Determination of fipronil and its metabolites in environmental water samples by meltblown nonwoven fabric‐based solid‐phase extraction combined with gas chromatography‐electron capture detection

“…[2,3]. In the past years, fipronil had been put into use in a large amount due to its high insecticidal activity and low toxicity to mammals [4][5][6][7]. However, some studies had shown that fipronil exhibited high toxicity and adverse effects on non-target beneficial insects such as butterflies, bees, dragonflies, and many aquatic organisms [4,[6][7][8][9][10].…”

“…In the past years, fipronil had been put into use in a large amount due to its high insecticidal activity and low toxicity to mammals [4][5][6][7]. However, some studies had shown that fipronil exhibited high toxicity and adverse effects on non-target beneficial insects such as butterflies, bees, dragonflies, and many aquatic organisms [4,[6][7][8][9][10]. Meanwhile, there was evidence to suggest that short-term intake of a large amount of fipronil can induce adverse effects on the human nervous system, while long-term intake of fipronil could induce adverse effects on the liver, kidney, thyroid, and other organs and tissues [5,11].…”