MIL-101(Cr) based d-SPE/UPLC-MS/MS for determination of neonicotinoid insecticides in beverages

ABSTRACT Neonicotinoids are a relatively new generation of insecticides that have been used for control of pests such as aphids, leafhoppers and whiteflies. This paper presents for the first time a determination of residues of four neonicotinoid insecticides (acetamiprid, thiamethoxam, thiacloprid and imidacloprid) in Chilean honey using QuEChERS extraction and UHPLC-MS/MS analysis. The limits of detection and quantification found for all analytes ranging from 0.34 to 1.43 μg kg-1 and from 0.30 to 4.76 μg kg-1, respectively. The extraction using QuEChERS method provided recoveries over 79% and the precision showed coefficient of variation lower than 20%. These data are in agreement with the international criteria that recommend general recovery limits of 70 - 120%. Of the 16 samples analyzed, in three honey samples neonicotinoids pesticides were detected. These three samples were collected from the same geographical area (Rengo). Fruit and grain production characterize the province of Rengo. The analysis of the botanical origin of these honeys showed the absence of pollen grains of crops and the majority presence of pollen grains of weeds such as Medicago sativa, Galega officinalis and Brassica rapa, which could be associated with crops. Although the residue levels found were low, the results also confirm the actual occurrence of a transfer of neonicotinoid insecticides from exposed honeybees into honey.

Download Full-text

Determination of neonicotinoid insecticides residues in bovine tissues by pressurized solvent extraction and liquid chromatography–tandem mass spectrometry

Journal of Chromatography B ◽

10.1016/j.jchromb.2010.11.008 ◽

2011 ◽

Vol 879 (1) ◽

pp. 117-122 ◽

Cited By ~ 55

Author(s):

Zhiming Xiao ◽

Xiaowei Li ◽

Xiaolin Wang ◽

Jianzhong Shen ◽

Shuangyang Ding

Keyword(s):

Mass Spectrometry ◽

Liquid Chromatography ◽

Solvent Extraction ◽

Tandem Mass Spectrometry ◽

Tandem Mass ◽

Neonicotinoid Insecticides ◽

Chromatography Tandem Mass Spectrometry ◽

Liquid Chromatography Tandem Mass ◽

Pressurized Solvent Extraction

Download Full-text

Sensitive Detection of Neonicotinoid Insecticides and Other Selected Pesticides in Pollen and Nectar Using Nanoflow Liquid Chromatography Orbitrap Tandem Mass Spectrometry

Journal of AOAC International ◽

10.5740/jaoacint.17-0412 ◽

2018 ◽

Vol 101 (2) ◽

pp. 367-373 ◽

Cited By ~ 5

Author(s):

David Moreno-González ◽

Jaime Alcántara-Durán ◽

Bienvenida Gilbert-López ◽

Miriam Beneito-Cambra ◽

Víctor M Cutillas ◽

...

Keyword(s):

Mass Spectrometry ◽

Liquid Chromatography ◽

Ion Source ◽

Tandem Mass ◽

Quechers Method ◽

Neonicotinoid Insecticides ◽

Orbitrap Mass Spectrometer ◽

Q Exactive ◽

Concentration Levels

Abstract In this work, a new method based on nanoflow LC with high-resolution MS was developed for the determination of eight pesticides in pollen and nectar samples, including neonicotinoid insecticides and other selected pesticides commonly found in bees and beeswax. Detection was undertaken with a hybrid quadrupole-Orbitrap mass spectrometer (Q Exactive™) equipped with a commercial nanospray ion source. The extraction of pesticides from pollen samples was performed by a modified micro-QuEChERS method scaled down to Eppendorf tubes, whereas nectar samples were simply diluted with a water–methanol (95 + 5, v/v) solution. Good linearity (>0.999 in all cases) was obtained between 0.05 and 500 µg/kg and between 0.04 and 400 µg/kg for pollen and nectar, respectively. Recovery rates in pollen ranged from 85 to 97%, with RSDs <12%. Matrix effect was evaluated and showed negligible effects for all studied pesticides. The lowest concentration levels tested and validated were 0.5 and 0.4 µg/kg for pollen and nectar matrixes, respectively. In addition, selected incurred samples were studied, obtaining several positive findings in pollen and nectar samples, demonstrating the sensitivity and applicability of the proposed method.

Download Full-text