Optimization and validation of ultrasound application with a low-temperature method to analyze organochlorine pesticides in smuggled cigarette tobacco.

This work presents the optimization and validation of a method to quantify organochlorine pesticides in tobacco samples from smuggled cigarettes using ultrasound application and low-temperature extraction. The combined approach was validated for 20 organochlorine pesticides, achieving recoveries between 73% and 116%, and a relative standard deviation of less than 20%. The method minimized the matrix effect in 65% of the organochlorine pesticides. The limits of detection and quantification varied from 2 to 60 ng g-1 and 120 to 190 ng g-1, respectively. The method was applied to the analysis of 18 brands of smuggled cigarettes. The organochlorine pesticides found in the samples were cis-chlordane (89%), p,p'-dichlorodiphenyldichloroethylene (DDD) and methoxychlor (78%), endosulfan sulfate (67%), heptachlor epoxide, and endosulfan II (61%). The concentrations of the organochlorine pesticides in this study were higher than those in a similar survey on cigarettes marketed in China. The ultrasound application and low-temperature extraction may be an efficient alternative to analyzing tobacco samples since it uses only one extraction solvent, requires low-cost equipment, does not require an additional clean-up step, reduces the environmental impact through minimal waste generation, and can detect low analyte concentrations.

Development, validation and matrix effect of a QuEChERS method for the analysis of organochlorine pesticides in fish tissue.

This study aims to develop and validate a method to determine OCPs in fish tissues, minimizing the consumption of sample and reagents, by using a modified QuEChERS along with ultrasound, d-SPE and gas chromatography with an electron capture detector (GC-ECD), refraining the pooling. Different factorial designs were employed to optimize the sample preparation phase. The validation method presented a recovery of around 77.3% and 110.8%, with RSD lower than 13% and the detection limits were between 0.24 and 2.88 µgkg-1, revealing good sensitiveness and accuracy. The method was satisfactorily applied to the analysis of tissues from different species of fish and OCPs residues were detected. The proposed method was shown effective to determine OCPs low concentrations in fish tissues, using small sample mass (0.5 g), making the sample analyses viable without the need for grouping (pool).