[Determination of sodium cyclamate in liquor by high performance liquid chromatography-tandem mass spectrometry with
Huiwen Fang1, Yuan Zhou, Yuepeng Lu
1Wuhan Product Quality Supervision and Inspection Institute, Wuhan 430048, China.
Abstract:
An accurate determination of quantitative and confirmative method for sodium cyclamate in liquor by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) with linear trap technology has been established. Without pretreatment, the sample was directly injected after filtering through a 0.2 microm micro filter. The HPLC separation was performed on an Atlantis dC18 column (150 mm x 2.1 mm, 3 microm) by gradient elution with methanol and water containing 0.1% (v/v) formic acid. The eluent was determined and confirmed in multiple reaction monitoring-enhanced product ion (MRM-EPI) scan mode. The acquired data from MRM for the quantitative determination, and the product ion spectra were used for library search for qualitative confirmatory analysis. External standard was used for the quantitative determination of sodium cyclamate in liquor, and good linearity (r = 0.9991) was obtained over the range of 1.320 - 132.0 microg/L. The limit of detection (LOD, S/N = 3) for sodium cyclamate was 0.1 microg/L. The average recoveries ranged from 96.38% to 107.2% at the spiked levels of 2.640, 26.40 and 100.0 microg/L with the relative standard deviations (RSDs) less than 9%. The matching degrees of the spectra for all positive samples were higher than 92%. The method is simple, accurate and efficient for the determination of sodium cyclamate in liquor and particularly suitable for confirmatory analysis of positive samples.
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