高效液相色谱法测定瓜子中糖精钠谱峰判定研究

Study on Determination of Saccharin Sodium in Melon Seeds by HPLC

针对在瓜子中糖精钠的液相色谱法测试过程中,容易出现的糖精钠假阳性问题,通过调整流动相比例,使样品中糖精钠谱峰和干扰谱峰分离,从而对样品中糖精钠进行准确的定性和定量。测试结果表明,采用GB5009.28—2016第一法,V(乙酸铵)∶V(甲醇)=95∶5时,瓜子样品的谱图中出现糖精钠干扰峰;调整流动相比例为V(乙酸铵)∶V(甲醇)=89∶11后,糖精钠谱峰与干扰峰分离完全。对样品进行回收率和精密度实验,糖精钠的回收率分别为99%,102.3%和102.2%,RSD分别为3.1%,2.3%和2.5%,能够满足检验要求。

Aiming at the false positive problem of saccharin sodium test in melon seeds by HPLC method,the spectrum peak of saccharin sodium and the interference spectrum peak were separated by adjusting the ratio of mobile phase,so that the saccharin sodium in the sample was accurately qualitatively and quantitatively determined.The results showed that using the first method of GB 5009.28—2016,saccharin sodium interference peak appeared in the spectrum of melon seed sample when the ratio of ammonium acetate to methanol was 95∶5.After adjusting the mobile phase ratio of ammonium acetate and methanol to 89∶11,the spectrum peak of saccharin sodium was completely separated from the interference peak.The recovery and precision experiments were carried out.The recoveries of saccharin sodium were 99%,102.3%and 102.2%,RSD were 3.1%,2.3%and 2.5%respectively,which met the test requirements.