Determination of Neonicotinoid Pesticides in Propolis with Liquid Chromatography Coupled to Tandem Mass Spectrometry

Autor: Helena Prosen, Ester Heath, Jernej Markelj, David Heath, Andreja Kandolf Borovšak, Rok Tomšič
Rok vydání: 2020
Předmět:
Insecticides
QuEChERS
Thiazines
Pharmaceutical Science
010501 environmental sciences
Quechers
01 natural sciences
Guanidines
Acetamiprid
Propolis
Article
Analytical Chemistry
lcsh:QD241-441
chemistry.chemical_compound
udc:543.544.5:543.51
Neonicotinoids
lcsh:Organic chemistry
neonikotinoidi
Limit of Detection
Tandem Mass Spectrometry
Drug Discovery
Physical and Theoretical Chemistry
LC-MS/MS
0105 earth and related environmental sciences
Chromatography
010401 analytical chemistry
Organic Chemistry
Selected reaction monitoring
Solid Phase Extraction
Neonicotinoid
Pesticide Residues
Clothianidin
Thiacloprid
Nitro Compounds
0104 chemical sciences
propolis
Thiazoles
chemistry
Chemistry (miscellaneous)
Calibration
Molecular Medicine
neonicotinoids
Thiamethoxam
SPE
Drug Contamination
Chromatography
Liquid
Zdroj: Molecules
Molecules, vol. 25, no. 24, 5870, 2020.
Molecules, Vol 25, Iss 5870, p 5870 (2020)
Volume 25
Issue 24
ISSN: 1420-3049
Popis: In this study, a method was developed for the determination of five neonicotinoid pesticides (acetamiprid, clothianidin, imidacloprid, thiacloprid, and thiamethoxam) in propolis. Two sample preparation methods were tested: solid-phase extraction and the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method. The identities of analytes were confirmed using liquid chromatography&ndash
tandem mass spectrometry (LC-MS/MS) in the selected reaction monitoring mode. Solid-phase extraction resulted in cleaner extracts
therefore, the SPE-LC-MS/MS method was validated according to the SANTE protocol in triplicate at two spiking levels (10 ng/g and 50 ng/g). The average recoveries of analytes ranged from 61% to 101%, except for clothianidin (10&ndash
20%). The LOD ranged from 0.2 ng/g to 4.4 ng/g, whereas the LOQ was in the range of 0.8 ng/g&ndash
14.7 ng/g. In order to compensate for the matrix effect, matrix-matched calibration was used. Good accuracy (relative error: 1.9&ndash
10.4%) and good linearity (R2 >
0.991) were obtained for all compounds. The optimised method was applied to 30 samples: 18 raw propolis and 12 ethanol tinctures. Acetamiprid, imidacloprid, and thiacloprid were detectable in seven samples but were still below the LOQ. This study is the first to report the determination of several neonicotinoid residues in propolis.
Databáze: OpenAIRE
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