Methodology for trace analysis of 17 pyrethroids and chlorpyrifos in foodstuff by gas chromatography–tandem mass spectrometry

• Published in: Analytical and bioanalytical chemistry Vol. 408; no. 27; pp. 7689 - 7697
• Main Authors: Dallegrave, Alexsandro, Pizzolato, Tânia Mara, Barreto, Fabiano, Eljarrat, Ethel, Barceló, Damià
• Format: Journal Article
• Language: English
• Published: Berlin/Heidelberg Springer Berlin Heidelberg 01-11-2016; Springer; Springer Nature B.V
• Subjects: Analytical Chemistry; Animal products; Animals; Biochemistry; Cattle; Characterization and Evaluation of Materials; Chemical properties; Chemistry; Chemistry and Materials Science; Chickens - metabolism; Chlorpyrifos; Chlorpyrifos - isolation & purification; Chromatography; Cypermethrin; Data recovery; Deltamethrin; Eggs - analysis; Extraction; Fish Products - analysis; Food; Food Analysis - methods; Food contamination; Food Contamination - analysis; Food Science; Gas chromatography; Gas Chromatography-Mass Spectrometry; Identification and classification; Insecticides; Insecticides - isolation & purification; Ionization; Laboratory Medicine; Mass spectrometry; Mathematical analysis; Methodology; Methods; Milk; Milk - chemistry; Monitoring/Environmental Analysis; Permethrin; Pesticide Residues - isolation & purification; Pesticides; Pyrethrins - isolation & purification; Pyrethroids; Red Meat - analysis; Research Paper; Scientific imaging; Solid Phase Extraction - methods; Tandem Mass Spectrometry; Toxicity; Trace analysis; Ultrasonic imaging; Brazil; Rio Grande do Sul Brazil; Pyrethroid analysis; Negative chemical ionization tandem mass spectrometry; Isomeric factor; Fat food
• ISSN: 1618-2642; 1618-2650
• DOI: 10.1007/s00216-016-9865-5

This study aimed to develop an efficient, sensitive, and reliable analytical method for trace analysis of 17 different pyrethroids and chlorpyrifos in the fatty content of animal products, including beef, chicken, eggs, fish, and milk. The method developed is based on an ultrasound extraction using lyophilized samples, a solid phase extraction cleanup with basic alumina and C18 cartridges in tandem, and analysis by gas chromatography coupled to tandem mass spectrometry in negative chemical ionization mode. Recovery values were in the range of 27–128 % with relative standard deviation always below 25 %, and chiral analysis of recovery data showed predominance of isomers of
cis
form over
trans
. Limits of detection (LODs) ranged from 0.002 to 6.43 ng g
−1
lipid weight (lw), and limits of quantification (LOQs) ranged between 0.006 and 21.4 ng g
−1
 lw. The developed methodology was used for the analysis of 25 samples of fatty foods. All samples were positive for at least one of the pesticides, chlorpyrifos, bifenthrin, cyhalothrin, permethrin, cypermethrin, or deltamethrin, with mass fraction levels ranging from 0.03 to 270 ng g
−1
lw.
Graphical Abstract
ᅟ