摘要
建立了白酒中安赛蜜、糖精钠、甜蜜素、三氯蔗糖、阿斯巴甜和纽甜6种甜味剂的高效液相色谱-串联质谱(HPLC-MS/MS)分析方法。白酒样品经微孔滤膜过滤后,以乙腈和含0.1%甲酸的水溶液为流动相,在ZORBAX Eclipse Plus C18色谱柱上进行分离,以电喷雾多反应监测(MRM)模式进行质谱分析。研究结果表明,6种甜味剂在检测范围内均具有良好的线性关系(R2〉0.997);方法的检出限LOD(S/N=3)分别为0.36μg/L、1.30μg/L、0.54μg/L、4.08μg/L、0.15μg/L和0.003μg/L,定量限LOQ(S/N=10)分别为1.21μg/L、4.34μg/L、1.80μg/L、13.61μg/L、0.49μg/L和0.01μg/L;样品的回收率分别为95.2%~97.5%、95.4%~98.7%、97.0%~97.8%、98.3%~100.7%、96.1%~99.9%和93.4%~98.6%;相对标准偏差分别为0.83~3.34、1.80~3.42、1.17~3.14、0.70~3.10、0.29~1.10和0.25~3.30。该分析方法前处理简单、灵敏度高、重现性好、分析速度快,可用于白酒中甜味剂的检测。
A rapid and accurate analytic method based on HPLC-MS/MS had been developed for the determination of six kinds of sweeteners in liquor, including acesulfame potassium, saccharin sodium, sodium cyclamate, sucralose, aspartame and neotame. Liquor samples underwent microporous membrane filtration, then separated on a ZORBAX Eclipse Plus C 18 column with acetonitrile and 0.1% formic acid aqueous solu- tion as the mobile phase, and then electrospray ionization was applied and operated in the multiple reaction monitoring (MRM) mode. The re- suits showed that, the correlation curves of six sweeteners showed good linearity (R2~0.997), the limits of detection (LOD, S/N=3) were 0.36 μg/L, 1.30 μg/L, 0.54 μg/L, 4.08 μg/L, 0.15 μg/L and 0.003 μg/L, respectively; the limits of quantitation (LOQ, S/N=10) were 1.21 μg/L, 4.34 μg/L, 1.80 μg/L, 13.61 μg/L, 0.49 μg/L and 0.01 μg/L, respectively; and the recoveries were 95.2 %-97.5 %, 95.4 %-98.7 %, 97.0 %-97.8 %, 98.3 %-100.7 %, 96.1%-99.9 % and 93.4 %-98.6 %, respectively; the relative standard deviations (RSD) were 0.83-3.34, 1.80- 3.42, 1.17-3.14, 0.70-3.10, 0.29-1.10 and 0.25 -3.30, respectively. The method was sensitive and reproducible with a simple pretreatment and rapid analysis speed, which could be applied to detect sweeteners in liquor.
出处
《酿酒科技》
2016年第3期122-124,共3页
Liquor-Making Science & Technology