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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-C_(18)(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 establish a rapid, accurate and sensitive solid phase extraction-RP-HPLC method for the simultaneous determination of 5 industrial dyes residues in raisins such as Acid Red 2G, Acid Red 14, Acid Yellow 73, Acid Orange 2 and Acid Blue 62 method. Methods The samples were purified by HLB solid phase extraction with ammonia-methanol-water (2:80:18, V / V) as the extract. The samples were eluted with 0.1% formic acid aqueous solution and methanol solution containing 2% After the nitrogen gas was evaporated to dryness and initial volume of the mobile phase was reached, the mobile phase was eluted with acetonitrile-0.02 mol / L ammonium acetate solution (10:90, V / V) on a ZORBAX SB-C 18 (4.6 mm × 250 mm, V) as mobile phase, using gradient elution separation, UV detector variable wavelength detection, external standard quantitative. Results Five industrial dyes, Acid Red 2G, Acid Red 14, Acid Yellow 73, Acid Orange 2 and Acid Blue 62, all showed good linearity in the range of 0.50 ~ 50 mg / L. The recoveries of the five analytes were 86.0 % ~ 110.2%, RSD less than 6%, the lowest limit of detection was 0.5 mg / kg. Conclusion This method is simple, sensitive, reproducible, and can meet the needs of industrial testing of raisins residue.