Citation: FENG Biting, GAN Zhiwei, HU Hongwei, SUN Hongwen. Optimization of sample pretreatment method for the determination of typical artificial sweeteners in soil by high performance liquid chromatography- tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2014, 32(9): 930-935. doi: 10.3724/SP.J.1123.2014.05033 shu

Optimization of sample pretreatment method for the determination of typical artificial sweeteners in soil by high performance liquid chromatography- tandem mass spectrometry

1.
Key Laboratory of Pollution Processes and Environmental Criteria of Ministry of Education, Nankai University, Tianjin 300071, China

Corresponding author: SUN Hongwen,
Received Date: 22 May 2014
Available Online: 26 June 2014
Fund Project: 国家杰出青年基金项目(41225014) (41225014)国家“973”计划项目(2014CB441104). (2014CB441104)

The sample pretreatment method for the determination of four typical artificial sweeteners (ASs) including sucralose, saccharin, cyclamate, and acesulfame in soil by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was optimized. Different conditions of extraction, including four extractants (methanol, acetonitrile, acetone, deionized water), three kinds of ionic strength of sodium acetate solution (0.001, 0.01, 0.1 mol/L), four pH values (3, 4, 5 and 6) of 0.01 mol/L acetate-sodium acetate solution, four set durations of extraction (20, 40, 60, 120 min) and number of extraction times (1, 2, 3, 4 times) were compared. The optimal sample pretreatment method was finally set up. The samples were extracted twice with 25 mL 0.01 mol/L sodium acetate solution (pH 4) for 20 min per cycle. The extracts were combined and then purified and concentrated by CNW Poly-Sery PWAX cartridges with methanol containing 1 mmol/L tris(hydroxymethyl) amino methane (Tris) and 5%(v/v) ammonia hydroxide as eluent. The analytes were determined by HPLC-MS/MS. The recoveries were obtained by spiked soil with the four artificial sweeteners at 1, 10, 100 μg/kg (dry weight), separately. The average recoveries of the analytes ranged from 86.5% to 105%. The intra-day and inter-day precisions expressed as relative standard deviations (RSDs) were in the range of 2.56%-5.94% and 3.99%-6.53%, respectively. Good linearities (r²>0.995) were observed between 1-100 μg/kg (dry weight) for all the compounds. The limits of detection were 0.01-0.21 μg/kg and the limits of quantification were 0.03-0.70 μg/kg for the analytes. The four artificial sweeteners were determined in soil samples from farmland contaminated by wastewater in Tianjin. This method is rapid, reliable, and suitable for the investigation of artificial sweeteners in soil.
- high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS),
- artificial sweeteners,
- soil,
- sample pretreatment method,
- optimization
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沈阳化工大学材料科学与工程学院沈阳 110142