Citation: HUANG Huiqiu, HUANG Lilai, XIA Ping. Simultaneous determination of methylmercury and inorganic arsenics in aquatic products by gas chromatography-mass spectrometry with aqueous derivatization[J]. Chinese Journal of Chromatography, ;2016, 34(9): 918-924. doi: 10.3724/SP.J.1123.2016.04032 shu

Simultaneous determination of methylmercury and inorganic arsenics in aquatic products by gas chromatography-mass spectrometry with aqueous derivatization

1.
Pingyang County Center for Disease Prevention and Control, Wenzhou 325400, China;
2.
Food and Drug Inspection and Testing Center of Pingyang County, Wenzhou 325400, China

Received Date: 20 April 2016

A fast analytical method based on gas chromatography-mass spectrometry (GC-MS) with aqueous derivatization was established for the simultaneous determination of methylmercury and inorganic arsenics in aquatic products. Methylmercury and inorganic arsenics in samples were extracted with hydrochloric acid (6 mol/L) by ultrasonic extraction. After centrifugation at -10℃, inorganic arsenics (As³⁺ and As⁵⁺) were derivatized under 35℃ water bath for 30 min with 2,3-dimercapto-1-propanol (BAL), then the derivative and methylmercury were extracted with toluene. The non-fatty components in the hydrochloric acid extract were avoided to get into the toluene by adding absolute ethanol before extraction, so the tested solution was purified. Then sodium tetraphenylborate solution (pH 3.6) was added to toluene extraction solution as the derivatization reagent. After centrifugation, the derivatives in organic phase were determined by GC-MS with selected ion monitoring (SIM) mode, and quantified with external standard method. The results showed that the calibration curves were linear in the range of 5-2000 μg/L for methylmercury and inorganic arsenic with correlation coefficients (r) greater than 0.999, and the limits of detection (LODs) were 0.7-3 μg/kg (S/N=3). The recoveries were 80.0%-110.0% at three spiked levels (10, 100, 1000 μg/kg), and the relative standard deviations (RSDs) were 2.5%-9.4% (n=6). The new method is simple, accurate and sensitive, and it has been successfully applied to the determination of methylmercury and inorganic arsenics in real aquatic products for the risk monitoring of food pollutants.
- gas chromatograph-mass spectrometry (GC-MS),
- aqueous derivatization,
- methylmercury,
- inorganic arsenics,
- aquatic products
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1.
沈阳化工大学材料科学与工程学院沈阳 110142