超高压液相色谱—质谱同时测定白酒中6种微量甜味剂的方法研究

Ultra-High Pressure Liquid Chromatography-Mass Spectrometry Method for Simultaneous Determination of Six Micro-Sweeteners in Distilled Spirit

DOI：

中文关键词: 超高压液相色谱—质谱联用 甜味剂 白酒

英文关键词: UPLC-MS sweeteners distilled spirit

基金项目:国家“十一五”科技支撑计划项目(2007BAK36B06)

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中文摘要:

为了检测白酒中6种甜味剂(安赛蜜、糖精钠、甜蜜素、三氯蔗糖、阿斯巴甜、纽甜),建立了一种超高压液相色谱质谱联用的新方法。样品预处理后,通过BEH C-18色谱柱分离,以甲醇-20 mmol/L乙酸铵水溶液为流动相进行梯度洗脱,在ESI负离子模式下检测,一次进样分析仅需10 min。以优化后的条件进行测定,6种甜味剂线性范围均在0.05~5.0 mg/L内,线性相关系数均大于0.994 5。得到安赛蜜检出限为0.05 mg/L、糖精钠、甜蜜素、纽甜检出限为0.01 mg/L、三氯蔗糖、阿斯巴甜检出限为0.1 mg/L。加标水平为0.5 mg/L和1.0 mg/L时,回收率在86.48%~116.90%之间,相对标准偏差为0.22%-3.90%。方法准确可靠、简便快速、可达到同时检测6种甜味剂的目的。

英文摘要:

In this manuscript,a novel ultra performance liquid chromatography(UPLC) coupled with mass spectrometry(MS) method was developed for the simultaneous determination of six micro-sweeteners(acesulfame-K,saccharin sodium,sodium cyclamate,sucralose,aspartame,neotame) in distilled spirit.After sample preparation,the analytes was seperated on an BEH C-18 column with methanol-20 mM ammonium acetate as mobile phase for gradient elution and detected at electrospray ionisation(ESI) source operating in negative mode,along with the accurate mass of their main fragment ion.It takes only 10 minutes to finish a whole seperation and detection.Under the optimized conditons the six compounds behave linearly in the 0.05-5.0 mg/L concentration range,with correlation coefficient >0.9945.The detection limits is 0.05 mg/L for acesulfame-K,0.01 mg/L for saccharin sodium,sodium cyclamate,neotame and 0.1 mg/L for sucralose,aspartame.The recoveries at the tested concentrations of 0.5 and 1.0 mg/L were 86.48 %～116.90 %,with the relative standard deviations of 0.22 %～3.90 %.The method has been successfully applied to simultancously detect six synthetic sweeteners in distilled spirit samples and illustrated accurate and effective.

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