摘要
目的:建立离子色谱法检测食品添加剂焦碳酸二甲酯(DMDC)中的杂质氯离子。方法:样品用水溶解超声定容后,采用SH-AC-1阴离子交换柱(25 cm×4.6 mm,7μm)分离,抑制电导法检测。分别选用碳酸钠,四硼酸钠为淋洗液。考察了淋洗液种类,浓度对氯离子与干扰离子的分离度的影响。最佳色谱条件为:采用0.005 mol/L的四硼酸钠水溶液作为淋洗液,流速1.0 mL/min。结果:在此条件下,样品中的氯离子可以和其他的干扰离子分离,而且分离度达3.0以上,峰形对称。在(0.1～ 5.0 mg/L)范围内,可获得良好的线性关系,线性相关系数大于0.999;氯离子检出限(S/N=3)达(0.007 mg/L),加标回收率达97.5%以上,重现性好。结论:该方法简便快速灵敏准确,可以用于食品添加剂DMDC中氯离子测定。
Objiective： To establish a method for the determination of chloride ion in DMDC （dimethyl dicarbonate） as food additives by ion exchange chromatography. Method： Sample was dissluted by water after ultrasonic, chromatographic separation was performed on a SH-AC-1 （25 cm×4.6 mm, 5μm） anion exchange column, Suppressed conductivity detection. Using sodium carbonate, sodium borate as the eluent, respectively. The effects of the types of eluent, eluent concentration on separation of chloride ion and interfering ion were investigated. The optimized chromatographic conditions for the determination of the chloride were as follows： 0.005 mol/L of sodium borate solution as eluent and flow rate of 1.0 mL/min. Results： Under these conditions, the chloride ions and other interfering ion can be completely separated in the sample, the resolution of peak attained 3.0 or more and the symmetry of peaks was better. The good linear calibration curve were obtained for the range of 0.1-5.0 mg/L with the linear relative coefficient more than 0.999, chloride ion detection limit（SIN：3） was 0.007 mg/L, The standard added recoveries were above 97.5% with good reproducibility. Conclusion： The method is simple, rapid, sensitive and accurate, It is suitable for determination of chloride ions in DMDC as food additives.
出处
《食品科技》
CAS
北大核心
2012年第2期291-293,共3页
Food Science and Technology
基金
科技部科技型中小企业技术创新基金(09C26213711749)
