Rapid QuEChERS Approach Using Novel Solid Phase Extraction for Insecticides in Lobster and Shellfish Tissue with Gas Chromatography–Tandem Mass Spectrometry

Abstract

Novel, rapid, inexpensive, and simple QuEChERS extraction followed by phospholipid solid phase extraction was successfully developed and validated for the determination of methoprene, resmethrin, bifenthrin, cyhalothrin, and permethrin in lobster and shellfish tissues by gas chromatography–tandem mass spectrometry. This method is equivalent in final sample purity to the traditional gel permeation and open column chromatography sample preparation techniques, but has clear advantages due to reductions in time, labor, solvent use, and can be performed with minimal staff training. The proposed methodology was effectively applied to the analysis of North Atlantic lobster (hepatopancreas and muscle) and shellfish tissue. The linearity of the calibration curves for all analytes were R² > 0.9991. The surrogate recoveries were 98.2 ± 18.0%, while the target compound recoveries, for fortified samples, were in the range of 62.0%–128.8% with RSD values <17.2% for all compounds. The detection limits for the analytes ranged from 0.0056 µg/g to 0.76 µg/g with 84.4–119.5% accuracy and relative standard deviations less than 3.77%.

Keywords:

• Gas chromatography–mass spectrometry
• GC-MS/MS
• Insecticides
• Lobster
• QuEChERS
• Shellfish

ACKNOWLEDGMENTS

We acknowledge valuable assistance provided by Jennifer Burgess, Kendon Graham, Steve Harrington, and Kim Lilley of Waters Corporation (USA) and Jay Oakley of GeneVac (UK). Special thanks to Gary Ulatowski of University of Connecticut who provided invaluable assistance during the method development and sample preparation.

Notes

*Mass used for all samples is 0.5 g; concentration factor is 10.

^a Zulkosky et al. 2005: 10 mL of water sample; liquid–liquid extraction; 100× concentration factor; LC-TOF-MS.

^b De Guise et al. 2005: 2 g of lobster tissue, modified EPA 616 method, GC–MS.

^c Tong et al. 2013: 2 g of flos chrysanthemi extracted with 40 mL of acetonitrile; 40× concentration factor; GC-MS-MS.

†The values are estimated based on the lowest 0.5 ng/mL concentration standard with no actual statistical analysis performed.

*The same surrogate compound is used for all the insecticides; therefore, only one value is presented.

HP, hepatopancreas; ND, not detected; CV, calibration verification.

MS, matrix spike; HP, hepatopancreas.

Color versions of one or more of the figures in the article can be found online at www.tandfonline.com/lanl.