目的建立一种简便、快速的葡萄酒中安赛蜜、糖精、甜蜜素、阿斯巴甜、甜菊糖苷和纽甜的分散固相萃取-液相色谱/串联质谱(dSPE—UFLC-MS/MS)定性定量分析方法。方法样品以新型磁性纳米材料为吸附剂进行分散固相萃取,利用UFLC.ESI.MS/MS进行分离和串联质谱测定,采用保留时间结合三离子定性原则进行确证。结果磁性纳米材料是一种高效的分散固相萃取吸附剂,可有效去除葡萄酒中的干扰基质;电喷雾电离可获得稳定可靠的二级质谱裂解碎片离子,安赛蜜、糖精、甜蜜素、阿斯巴甜、甜菊糖苷和纽甜的定量离子对分别为m/z162→82、m/z182→42、m/z178→80、m/z293→200、m/z803→641、m/z 377→200,6种甜味剂的精密度范围为1.1%~4.0%,回收率范围为83.4%~104.0%,定量检出限范围为0.1~5.0μg/L。结论建立的方法快速、灵敏、准确,适用于葡萄酒中安赛蜜、糖精、甜蜜素、阿斯巴甜、甜菊糖苷和纽甜的含量确证分析。
Objective To develop a rapid and simple qualitative and quantitative method for determination of acesulfame, saccharin, cyclamate, aspartame, stevioside and neotame in wine by dispersive solid-phase extraction and ultra-fast liquid chromatography coupled with electrospray ionization tandem mass spectrometry (dSPE-UFLC-ESI/MS/ MS). Methods After the sample was extracted and cleaned by dispersive solid-phase extraction using novel magnetic nanomaterials as adsorbents, the separation was performed by UFLC and the cracking was used by the optimized ESI/MS/MS conditions in a negative electrospray ionization mode. Confirmatory detection was carried out by the principle of three qualitative ions and the retention time. Results The interference matrix could be effectively adsorbed by the novel magnetic nanomaterials. The MS/MS fragment ions were reliable and steady under the suitable conditions, the cracking ways to the parent ions and fragment ions were clear. Quantitative ion pairs were m/z 162→82 for acesulfame, m/z 182→42 for saccharin, m/z 178→80 for cyclamate, m/z 293→200 for aspartame, m/z 803→641 for stevioside, m/z 377→200 for neotame. The recoveries were between 83.4% and 104.0% with the relative standard deviations (RSDs) of 1.1% -4.0%. The limits of quantification (LOQs) were in the range of 0. 1 - 5.0 trg/L. Conclusion The established method was rapid, accurate and sensitive, it is suitable for confirmation for acesulfame, saccharin, cyclamate, aspartame, stevioside and neotame in wine.