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研究优化了超高效液相色谱串联质谱(UPLC-MS/MS)法检验腌制蔬菜样品中主要3种甜味剂前处理条件,建立了一种测定效果优良的UPLC-MS/MS法同时检验腌制蔬菜样品中3种甜味剂的途径。试验结果显示甲醇水溶液提取-超高效液相色谱串联质谱法同时测定腌制蔬菜产品中的3种甜味剂方法各较优参数为:pH 7的40%甲醇水溶液,提取料液比1︰3(g/m L),超声震荡提取15 min。提取样液测定采用ACQUITY UPLC BEH C_(18)(2.1 mm×50mm,1.7μm)色谱柱,乙腈-乙酸铵(1 mmol/L)溶液为流动相,流动相A为有机相,流动相B为水相,柱温40℃,进样量2μL;流速为0.5 m L/min梯度洗脱。在ESI负离子模式下,采用多反应监测g(MRM)模式进行MS/MS检测,3种待测成分在线性范围内有较好的线性关系,相关系数R均大于0.999,该方法下,安赛蜜、糖精钠和甜蜜素检出限(LOD)分别为18.99,7.63和11.27μg/L,定量限(LOQ)分别为58.67,22.96和35.01μg/L;安赛蜜、糖精钠和甜蜜素的加标回收率分别为98.44%~98.17%,99.35%~99.97%和96.58%~98.87%,相对标准偏差(RSD)均小于5%,该方法准确可靠。
The UPLC-MS / MS method was used to determine the pretreatment conditions of the three major sweeteners in the preserved vegetable samples, and a UPLC-MS / MS simultaneous determination method Ways to Preserve Three Kinds of Sweeteners in Vegetable Samples. The results showed that the optimal parameters for simultaneous determination of three kinds of sweeteners in salted vegetable products by aqueous methanol extraction and ultra performance liquid chromatography-tandem mass spectrometry were as follows: 40% aqueous solution of methanol at pH 7, (g / m L) and sonicated for 15 min. The sample was extracted with ACQUITY UPLC BEH C 18 (2.1 mm × 50 mm, 1.7 μm) column and acetonitrile-ammonium acetate (1 mmol / L) solution as mobile phase. Mobile phase A was organic phase and mobile phase B was Water phase, the column temperature 40 ℃, injection volume 2μL; flow rate of 0.5 m L / min gradient elution. In the ESI negative ion mode, MS / MS was carried out by using MRM mode. The three analytes had a good linear relationship in the linear range with the correlation coefficient R greater than 0.999. In this method, The detection limits (LOD) of honey, sodium saccharinate and sodium cyclamate were 18.99, 7.63 and 11.27 μg / L, respectively, and the LOQs were 58.67, 22.96 and 35.01 μg / L, respectively. The spiked recoveries were 98.44% -98.17%, 99.35% -99.97% and 96.58% -98.87%, respectively. The relative standard deviations (RSDs) were less than 5%. The method was accurate and reliable.