离子对反相高效液相色谱法测定液态奶中硫氰酸根的含量  

Ion-Pair RP-HPLC Determination of Thiocyanate in Liquid Milk

作　　者：陈世奇 邓美林 朱永红 屠大伟 

机构地区：[1]重庆市计量质量检测研究院,重庆401121

出　　处：《理化检验（化学分册）》2012年第9期1078-1080,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：采用离子对反相高效液相色谱法测定液态奶中硫氰酸根的含量。样品经乙腈提取后,用Zorbax Extend C18(150mm×4.6mm,5μm)作固定相,以含3mmol.L-1四丁基溴化铵的磷酸盐缓冲溶液与甲醇以体积比70比30组成的混合溶液为流动相,对试液进行离子对色谱分离。于波长231nm处用紫外检测器进行测定。硫氰酸根的质量浓度在0.4～50.0mg.L-1之间与峰面积呈线性关系,方法的检出限(3S/N)为0.055mg.L-1,测定下限(10S/N)为0.18mg.L-1。方法用于液态奶样品分析,加标回收率在92.0%～102%之间;测定值的相对标准偏差(n=6)在2.53%～4.86%之间。The content of thiocyanate in liquid milk was determined by ion-pair RP-HPLC. The sample was extracted by acetonitrile, and the sample solution obtained was separated on Zorbax Extend C18 column （150 min×4.6 mm, 5 μm） with a mixture of phosphate buffer solution （containing 3 mmol ·L-1 tetrabutylammonium bromide） and methanol in the ratio 70 to 30 by volume as mobile phase, and detected at 231nm by UV-detector. Linear relationship between values of peak area and mass concentration of thiocyanate was kept in the range of 0. 4-- 50.0 mg·L-1 with detection limit （3S/N） of 0. 055 mg·L-1 and lower limit of determination （10S/N） of 0. 18 mg ·L-1. The proposed method was applied to the analysis of liquid milk. Tests for recovery and precision were made by standard addition method, giving values of recovery and RSD＇s （n = 6） in the ranges of 92. 0%- 102% and 2.53%--4. 86% respectively.

关 键 词：离子对反相高效液相色谱法 硫氰酸钠 液态奶 

分 类 号：O652.63[理学—分析化学]