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Yin F.,State Non Staple Food Quality Supervision and Test Center | Ding Z.,State Non Staple Food Quality Supervision and Test Center | Cao X.,State Non Staple Food Quality Supervision and Test Center | Gao J.,State Non Staple Food Quality Supervision and Test Center | And 4 more authors.
Chinese Journal of Chromatography (Se Pu) | Year: 2011

A solid phase extraction-high performance liquid chromatography/electrospray ionization-tandem mass spectrometry (SPE-HPLC/ESI-MS/MS) method for the determination of 3 sweeteners (acesulfame (AX), sodium saccharin (SA), sodium cyclamate (SC)) in vinegars has been developed. The sample was diluted with acidic water, then purified and enriched with a weak anion exchange SPE column. The HPLC separation was performed on a Pursuit C18 column (150 mm × 2. 0 mm, 3 μm) by gradient elution with 10 mmol/L ammonium acetate containing 0. 1% (v/v) ammonia water and acetonitrile as the mobile phases. The analytes were detected by ESI --MS/MS in multiple reaction monitoring (MRM) mode to satisfy qualitative and quantitative detections. Good linearities (r 2 > 0. 99) were obtained over the range of 0. 01-0. 50 mg/L. The limits of quantification (LOQs) for SA, AK and SC were 10, 5 and 5 μg/kg, respectively. The average recoveries ranged from 72. 1% to 96. 8% at the spiked levels of 0. 01 and 0. 1 mg/L with the relative standard deviations (RSDs) less than 15%. This method is accurate, highly sensitive for qualitative and quantitative analysis of the 3 sweeteners in vinegars. Source


Yin F.,State Non Staple Food Quality Supervision and Test Center | Ding Z.,State Non Staple Food Quality Supervision and Test Center | Yang Z.,State Non Staple Food Quality Supervision and Test Center
Chinese Journal of Chromatography (Se Pu) | Year: 2012

Rhodamine B (RB), as an unlawful colour, is forbidden to add into foods by Chinese government. A solid phase extraction-high performance liquid chromatography-tandem mass spectrometry (SPE-HPLC-MS/MS/method for the determination of RB in spices has been developed. The sample was extracted by acetonitrile and then centrifugated, purified and enriched with a strong positive ion exchange SPE column (Bond Elut Plexai PCX SPE column) after adding 10 mL 1% trichloroacetic acid solution. The HPJaC separation was performed on a Pursuit C18 column (100 mm × 2. 0 mm, 3 μm) by gradient elution with 0. 1% (v/v) formic acid solution and methanol as the mobile phase. The analyte was detected by electrospray ioni-zation in positive ion mode-MS/MS in multiple reaction monitoring (MRM) mode. The good linearity (R2 > 0. 99) was obtained over the range of 0. 6-6 μg/L. The limit of quantification (LOQ) for RB was 1. 2 μg/kg. The average recoveries were ranged from 80% to 121% at the spiked levels of 1. 197, 2.992 and 5.985 μg/L, and the relative standard deviations (RSDs) were not more than 15%. The conditions of mobile phase elution gradients; extraction solvents; and SPE columns were.optimized. This method is highly selective and has weak matrix effect for qualitative and quantitative analyses of RB in spices. Source

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