摘要:
建立高效液相色谱测定食品包装用胶黏剂中枞酸、新枞酸、去氢枞酸、长叶松酸和左旋海松酸的分析方法.对样品前处理和色谱分析条件进行了优化,以乙酸乙酯为溶剂,甲醇沉淀高聚物离心后微孔滤膜过滤,乙腈-0.4%乙酸水(80∶20)为流动相,流速为1.0 mL/min,等度洗脱,采用Venusil MP C18(2)色谱柱,二极管阵列检测器(DAD),高效液相色谱法测定,枞酸和新枞酸的检测波长为240 nm,长叶松酸和左旋海松酸为270 nm,去氢枞酸为208 nm,以外标法定量.结果表明,5种树脂酸的定量下限为2.5~ 10.0 mg/kg,线性范围跨越两个数量级以上,连续6次进样的相对标准偏差(RSD)不大于3.4%,加标回收率为92.2%~103.6%.该方法操作简单、干扰因素少、分析速度快,满足食品包装用胶黏剂中5种树脂酸的检测要求.%A high performance liquid chromatographic (HPLC) method was developed for the determination of 5 resin acids,including abietic acid,neoabietic acid,dehydroabietic acid,palustric acid and levopimaric acid in food contact adhesives.The conditions of sample pretreatment and chromatographic separation were optimized.The sample was dissolved with ethyl acetate,and the polymer was precipitated with methanol.After filtration with filter membrane,the extract was separated on a Venusil MP C1s(2) column with acetonitrile-0.4% acetic acid(80 ∶ 20) as mobile phase at a flow rate of 1.0 mL/min,detected accurately by HPLC with diode-array detector(DAD) at 240 nm for abietic acid and neoabietic acid,270 nm for palustricacid and levopimaric acid,208 nm for dehydroabietic acid,and quantified by the external standard method.The HPLC method showed a good linearity above two orders of magnitude,with detection limits of 2.5-10.0 mg/kg.The RSDs for 5 resin acids were no more than 3.4%,and the recoveries were in the range of 92.2%-103.6%.The method has the advantages of simple operation,rapid analysis and less interference factors,and could provide credible analysis for 5 resin acidsin food contact adhesives.