固相萃取-高效液相色谱-可变波长检测法同时测定调味品中甜味剂和人工合成色素

建立了同时测定调味品中糖精钠和合成色素的固相萃取-高效液相色谱(SPE-HPLC)分析方法。样品经石油醚低温去除油脂,聚酰胺固相萃取柱净化和富集,然后进行HPLC分析。采用反相C₁₈色谱柱,以甲醇和0.02 mol/L醋酸铵为流动相进行梯度洗脱,使用可变波长分别在230、510、484和510 nm进行检测。实验结果表明:糖精钠与合成色素的分离效果良好,回收率为88.6%～97.1%,相对标准偏差小于5%;方法检出限均可达到0.05 mg/kg。该方法操作简单,结果准确可靠,重现性好,适用于大批量调味品中甜味剂和人工合成色素的同时检测。

Simultaneous determination of saccharin sodium and synthetic colours in flavourings by solid phase extraction and high performance liquid chromatography

A method for the simultaneous determination of saccharin sodium and synthetic colours in flavourings by solid phase extraction (SPE) and high performance liquid chromatography with variable wavelengths was established. After degreased with petroleum ether, extracted, purified with SPE, and concentrated, the sample was separated on a C₁₈ column with a gradient elution of 0.02 mol/L ammonium acetate and methanol, and detected at 230, 510, 484 and 510 nm, separately. The saccharin sodium and synthetic colours were separated with this method. The recoveries were 88.6%-97.1% with the RSD<5%. The limit of detection was 0.05 mg/kg for all the analytes. The proposed method is simple, reliable and reproducible, and especially suitable for a lot of sample detections of saccharin sodium and synthetic colours in flavourings.