高效液相色谱法检测压敏胶及其制品中的防老剂D

Determination of Antioxidant D in Pressure-sensitive Adhesive and Its Products by High Performance Liquid Chromatography

建立了高效液相色谱法测定压敏胶及其制品中防老剂D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,甲醇为沉淀剂,乙腈-水(90∶10)为流动相,流速为0.5 mL/min,等度洗脱。采用C18色谱柱,二极管阵列检测器(DAD),高效液相色谱法测定,检测波长为310 nm,外标法定量。并建立了防老剂D的液相色谱-质谱确证方法。结果表明,防老剂D的质量浓度在0.01～1 mg/L和1～100 mg/L范围内与其色谱峰面积呈良好线性;方法的定量下限为1 mg/kg;在乳液型、热熔型、溶剂型3种压敏胶中的加标回收率为96%～100%,相对标准偏差(RSD)为1.1%～3.1%。方法简单、快速、灵敏,满足压敏胶及其制品中防老剂D的分析要求。

A high performance liquid chromatographic（HPLC） method was developed for the determination of antioxidant D in pressure sensitive adhesive and its products.The sample was dissolved with ethyl acetate,then precipitated by methanol.The extract was centrifugally separated for 5 min at a speed of 3 000 r/min.After filtrated with filter membrane,the supernatant was separated on a C18 column by isocratic elution using acetonitrile-water as mobile phase at a flow rate of 0.5 mL/min,and determined by HPLC with diode-array detector（DAD）at 310 nm,quantified by the external standard method.The conditions of sample pretreatment and chromatographic separation were optimized,and the confirmatory method of mass spectrometry used to quantitatively determine antioxidant D in the sample was established.Under the optimal conditions,the method showed good linearities between peak areas and the contents in the ranges of 0.01-1 mg/L and 1-100 mg/L for antioxidant D,with a limit of quantitation of 1 mg/kg.The established method was applied in the determination of antioxidant D in emulsion-type pressure-sensitive adhesive,hotmelt-type pressure-sensitive adhesive and solvent-type pressure-sensitive adhesive,and the spiked recoveries ranged from 96% to 100% with relative standard deviations（RSDs） of 1.1%-3.1%.The results indicated that this method was reliable,sensitive and repeatable,and could meet the requirement for analysis of antioxidant D in the pressure sensitive adhesive and its products.