Determination of Organotin Compounds in Wine by Microwave-Assisted Extraction and High Performance Liquid Chromatography–Inductively Coupled Plasma Mass Spectrometry

Abstract

A new analytical procedure for the determination of five organotin compounds in several matrix wine samples is reported. The organotin compounds were extracted by microwave-assisted extraction with n-hexane. Extraction conditions, such as volume of n-hexane required, extraction temperature, and extraction time, were investigated and optimized by an orthogonal array experimental design. The determination of organotin compounds in the final extracts was carried out by liquid chromatography–inductively coupled plasma mass spectrometry. The procedure showed limits of detection between 0.029–0.049 µg · L⁻¹. The linearity was in the range of 0.5 to 100 µg · L⁻¹. The precision expressed as relative standard deviation (RSD) was below 9.43%. The developed method was successfully employed to analyze different matrix wine samples, and some analytes were detected at the level of 0.053 to 1.14 µg · L⁻¹.

Keywords:

• Liquid chromatography–inductively coupled plasma mass spectrometry
• Microwave-assisted extraction
• Organotin compounds
• Wine

Acknowledgments

The financial support of this study from the National Key Technology R & D Program of the “12th Five-Year Plan” (2012BAK17B02), the Natural Science Foundation of China (20965005), and the Research Program of State Key Laboratory of Food Science and Technology of Nanchang University (SKLF-ZZB-201304) are gratefully acknowledged.

Notes

FBTO: fenbutatin oxide; MBT: monobutyltin; TeBT: tetrabutyltin; TMT: Trimethyltin. MSPD: Matrix solid-phase dispersion; SPME: solid-phase microextraction; LLE: liquid–liquid shaking extraction; UAE: ultrasound-assisted extraction.

^a Data were shown as mean ± SD (n = 3).

^a Factor A, volume of n-hexane: level 1, 10 mL; level 2, 15 mL; level 3, 20 mL.

^b Factor B, extraction time: level 1, 5 min; level 2, 10 min; level 3, 15 min.

^c Factor C, temperature: level 1, 60°C; level 2, 80°C; level 3,100°C.

K_i, mean effect of each factor at level i (i = 1, 2, 3).

^a ND: not detected (<LOD).

^b Data were shown as mean ± SD.