固相萃取-反相高效液相色谱法同时测定葡萄干中5种工业染料  

Simultaneous determination of five industrial dyes in raisins by solid phase extraction and high performance liquid chromatography

作　　者：杨毅华[1] 徐明敏[1] 陈波[1] 杨笑[1] 

机构地区：[1]宁波市北仑区疾病预防控制中心,浙江宁波315800

出　　处：《中国食品卫生杂志》2016年第1期52-56,共5页Chinese Journal of Food Hygiene

基　　金：浙江省微量有毒化学物与健康风险评估技术研究重点实验室开放基金项目(2014003);浙江省医药卫生科研项目(2013KYA187)

摘　　要：目的建立快速、准确、灵敏的固相萃取-反相高效液相色谱法同时测定葡萄干中酸性红2G、酸性红14、酸性黄73、酸性橙2和酸性蓝62等5种工业染料残留的检测方法。方法样品以氨水-甲醇-水（2∶80∶18,V/V）作为提取液,利用HLB固相萃取柱进行净化,采用0.1%甲酸水溶液淋洗,含2%氨水的甲醇溶液洗脱,氮吹挥干后用初始流动相定容,在ZORBAX SB-C18（4.6 mm×250 mm,5μm）色谱柱上,以乙腈-0.02 mol/L醋酸铵溶液（10∶90,V/V）为流动相,采用梯度洗脱分离,紫外检测器变波长检测,外标法定量。结果酸性红2G、酸性红14、酸性黄73、酸性橙2、酸性蓝62等5种工业染料在0.50-50 mg/L范围内均具有良好的线性,5种待测物的回收率在86.0%-110.2%,RSD均小于6%,最低定量检出限为0.5 mg/kg。结论本方法简便、灵敏、重现性好,能满足葡萄干中工业染料残留的实际检测工作需要。Objective To develop a rapid,accurate and sensitive method for the simultaneous determination of five industrial dyes（ acid red 2G,acid red 14,acid yellow 73,orange 2 and acid blue 62） by solid phase extraction（ SPE） and high performance liquid chromatography. Methods Samples were extracted by ammonia-methanol-water（ 2 ∶ 80 ∶ 18,V / V）,and cleaned up by the HLB solid phase extraction column. The analytes were washed with 0. 1% formic acid,eluted with 5% ammonia-methanol and dried by nitrogen. The residue was dissolved with the initial mobile phase,and the solution was separated on a ZORBAX SB-C18（ 4. 6 mm × 250 mm,5μm） column by using acetonitrile-ammonium acetate solution as the mobile phase in gradient program. Detection was performed with UV detector of variable wave-length.Quantitative analysis was carried out by measuring peak area and comparing it with external standard. Results There was good linearity in the range of 0. 50-50 mg / L for the five dyes. Recoveries were in the range of 86. 0%-110. 2%,and the relative standard deviation（ RSDs） were lower than 6%. The limits of quantification（ LOQs） were in the range of0. 5 mg / kg. Conclusion This method is simple,sensitive and reproducible,which could be applied to the routine analysis.

关 键 词：高效液相色谱法 固相萃取 工业染料 违法添加 食品污染物 葡萄干 

分 类 号：O657.72[理学—分析化学] TS255.42[理学—化学]