Abstract
Multiresidual pesticide determination in a biological sample is essential for an immediate decision and response related to various pesticide intoxications. A rapid and simultaneous analytical method for 260 pesticides in human urine was developed and validated using liquid chromatography-tandem mass spectrometry (LC-MS/MS). High speed positive/negative switching electrospray ionization (ESI) mode was used, and scheduled multiple reaction monitoring (MRM) was optimized. Three versions of scaled-down QuEChERS procedures were evaluated, and the procedure using non-buffer reagents (magnesium sulfate and sodium chloride) and excluding cleanup steps was selected for optimum pesticide extraction. The limit of quantitation (LOQ) in this methodology was 10 ng/mL for each target pesticide, and correlation coefficient (r2) values of calibration curves were ≥0.988 (linearity range; 10–250 ng/mL). In accuracy and precision tests, the relative error ranges were −18.4% to 19.5%, with relative standard deviation (RSD) 2.1%–19.9% at an LOQ level (10 ng/mL), and −14.7% to 14.9% (RSD; 0.6%–14.9%) at higher concentrations (50, 150, and 250 ng/mL). Recovery range was 54.2%–113.9% (RSD; 0.3%–20.0%), and the soft matrix effect (range; −20% to 20%) was observed in 75.4% of target pesticides. The established bioanalytical methods are sufficient for application to biomonitoring in agricultural exposures and applicable in the forensic and clinic.
Highlights
Pesticides have been widely applied on farms for control of problematic weeds or harmful pests such as certain insects and fungi
Scheduled multiple reaction monitoring (MRM) for each target pesticide was optimized with the high-throughput triple quadrupole mass spectrometer
An average of 17.3 pesticides could be detected in a minute, the total analysis time for 260 pesticides was within only 15 min in a sample
Summary
Pesticides have been widely applied on farms for control of problematic weeds or harmful pests such as certain insects and fungi. The use of pesticides has contributed to the improvement of crop/livestock yields and quality, increased shelf life of produce, and prevention of harmful organisms from interfering in human activities and structures, from which secondary benefits such as national agricultural economic development, reduced maintenance costs, or quality of life improvement have followed [1]. Despite the considerable advantages of pesticides, unwanted side effects have followed. Pesticide intoxication resulting from intentional intake or misuse during cultivation is a major social problem. Gunnell and coworkers investigated the global distribution of suicide by pesticide and estimated that there are 258234 (plausible range from 233997 to 325907) suicides from pesticide poisoning each year, representing 30% (27% to 37%) of all suicides worldwide [2].
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