超高效液相色谱-串联质谱法测定塑料包装果汁饮料中10种苯并三唑类紫外吸收剂

本研究建立了同时测定塑料包装果汁饮料中10种苯并三唑类紫外吸收剂的超高效液相色谱-串联质谱（UPLC-MS/MS）分析方法。使用Waters Acquity UPLC BEH C18（100 mm×2.1 mm×1.7 μm）色谱柱分离目标物，以甲醇和0.1%甲酸水溶液为流动相进行梯度洗脱，在电喷雾正离子模式下，采用多反应监测（MRM）模式进行定性和定量分析。样品以甲醇 二氯甲烷（1∶1，V/V）为洗脱溶剂，经C18固相萃取柱净化浓缩处理。结果表明，10种苯并三唑类紫外吸收剂在1~100 μg/L浓度范围内的线性关系良好，线性相关系数（R²）均大于0.996，方法定量限为0.1 μg/kg，阴性样品在2.5、5.0和25.0 μg/kg添加水平下的回收率介于79.8%~101.5%之间，相对标准偏差在1.0%~5.5%（n=6）之间。该方法准确、简便，可用于塑料包装果汁饮料中10种苯并三唑类紫外吸收剂的检测。

Simultaneous Determination of Ten Benzotriazole Ultraviolet Stabilizers in Plastic Bottled Fruit Juices Beverage by UPLC-MS/MS

A method was developed for the simultaneous determination of ten benzotriazole ultraviolet stabilizers in plastic bottled fruit juices beverages by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The separation was performed by using water containing 0.1% formic acid and methanol as the mobile phases with gradient elution at a flow rate of 0.3 mL/min. Qualitative and quantitative analysis were achieved after the chromatographic separation on a Waters Acquity UPLC BEH C18 column (100 mm×2.1 mm×1.7 μm). The electrospray ionization (ESI) source in positive ion mode was used of the analysis of the ten benzotriazole ultraviolet stabilizers in the multiple reaction monitoring (MRM) mode. The parameters were optimized, like as the effect of different solid-phase extraction (SPE) columns, elution solvents and elution volume. The condition of the final choice was that the sample was purified by C18 SPE column with 4 mL methanol-dichloromethane (1∶1, V/V). The standard curves are obtained with good correlation coefficients (R²>0.996) in their concentration range. The limit of quantification (LOQ, S/N=10) for the ten benzotriazole ultraviolet stabilizers is 0.1 μg/kg. The mean recoveries for the ten benzotriazole ultraviolet stabilizers at three spiked levels of 2.5, 5.0 and 25.0 μg/kg are 79.8%-101.5% with the relative standard deviations of 1.0%-5.5% (n=6). Ten kinds of food contacting materials were tested, benzotriazole ultraviolet stabilizer was not found in the sample. The method is accurate, simple and feasible for the simultaneous determination of benzotriazole ultraviolet stabilizers in plastic bottled fruit juices beverages.