摘要
建立了黄酒中甜蜜素残留的固相萃取-液相色谱/串联质谱法(SPE-LC/MS/MS)测定方法。黄酒样品用水稀释后,弱阴离子(WAX)固相萃取小柱净化,氨化甲醇洗脱。采用Hypersil Gold C18色谱柱(150 mm×2.1 mm,5μm),乙腈-0.1%甲酸水溶液为流动相,以电喷雾离子源负离子模式(MRM)定性、定量测定甜蜜素。甜蜜素在10～500μg/L范围内峰面积与质量浓度呈线性关系,相关系数为0.999 5。取有代表性的阴性样品进行添加回收试验,在0.5～5.0 mg/L范围内,回收率为81.1%～88.2%,相对标准偏差为3.65%～5.21%,方法的定量检测限为0.5 mg/L。该方法净化效果好,检测灵敏度高,能同时完成黄酒中甜蜜素的定量和定性分析。
A solid phase extraction -liquid chromatography / tandem mass spectrometry method for determiantion of sodium cyclamate was developed. The rice wine sample was diluted with ultra pure water, purified with WAX SPE coulmn, eluted with ammoniated methanol, then the sodium cyclamate in the sample was detected by LC-MS-MS in MRM mode using Hypersil Gold Cts column （ 150 mm × 2.1 mm, 5μm ） and acetonitrile-0.1% formic acid as mobile phase. The sodium cyclamate mass concentration was linear with peak area in the range of 10-500 μg / L, with the correlation coefficient of 0.999 5. The recoveries of sodium cyclamate spiked in samples at three levels ranged from 81.1% to 88.2% with the relative standard deviation of 3.65% -5.21%（n=5）. The limit of quantification was 0.5 mg/L. The method is sensitive and it can simultaneously complete quantification and qualitation analysis of sodium cyclamate in rice wine.
出处
《化学分析计量》
CAS
2012年第1期55-57,共3页
Chemical Analysis And Meterage
