液相色谱-串联质谱法测定食品接触材料及制品中新戊二醇迁移量

Determination of Neopentyl Glycol Migration in Food Contact Materials and Products by Liquid Chromatography-Tandem Mass Spectrometry

采用液相色谱-串联质谱(LC-MS/MS)建立了食品接触材料及制品中新戊二醇的测定方法。样品采用水、4%(体积分数,下同)乙酸、10%乙醇、20%乙醇、50%乙醇、95%乙醇和橄榄油作为食品模拟物进行迁移试验后,水、4%乙酸、10%乙醇浸泡液直接过滤进样,其他乙醇类模拟物浸泡液采用氮吹方式去除大部分乙醇后重新用水定容,橄榄油浸泡液采用10%乙醇萃取。经处理后的试液采用ACQUITY UPLC■BEH C_(18)(50 mm×2.1 mm,1.7μm)色谱柱,以0.01%甲酸溶液-乙腈为流动相进行梯度洗脱,在电喷雾离子源正离子(ESI+)多反应监测(MRM)模式下进行检测,外标法定量。在优化条件下,新戊二醇在10~100μg/L(μg/kg)范围内线性关系良好,相关系数大于0.999。在10、20、100μg/L(μg/kg)3个加标水平下,方法回收率为92.8%~117%,相对标准偏差(RSD)为0.90%~8.6%,检出限(LOD,S/N≥3)为5μg/L(μg/kg),定量下限(LOQ,S/N≥10)为10μg/L(μg/kg)。该方法具有前处理简单易行、灵敏度高、稳定可靠的优点,涉及的食品模拟物基本包括相关法规和标准中规定的类型,方法LOD和LOQ均低于相关法规和标准中的限量要求,能够满足食品接触材料及制品中新戊二醇迁移量的检测需求,为相关产品监管和质量控制提供了可靠的技术手段。

A liquid chromatography-tandem mass spectrometry(LC-MS/MS)was established for the determination of neopentyl glycol in food contact materials and products in this paper.Water,4%acetic acid(volume fraction),10%ethanol,20%ethanol,50%ethanol,95%ethanol and olive oil were used as the food simulants.After soaking in food simulants,different types of soaking solutions were pretreated with appropriate manners.Water,4%acetic acid and 10%ethanol soaking solutions were directly filtered and injected.For soaking solutions of other ethanol simulants,most of the ethanol was removed by nitrogen blowing in a certain volume,and water was used to replenish to the original volume.For olive oil soaking solution,10%ethanol was used for extraction.The separation was performed on an ACQUITY UPLC■ BEH C_(18)(50 mm×2.1 mm,1.7μm)chromatographic column by gradient elution,with 0.01%formic acid solution and acetonitrile as mobile phases.The detection was performed with electrospray ion source in positive ion(ESI+)multi reaction monitoring(MRM)mode.External standard method was used for quantitative determination.Under the optimized conditions,there was a good linear relationship for neopentyl glycol in the range of 10-100μg/L(μg/kg),with its correlation coefficient larger than 0.999.The spiked recoveries for neopentyl glycol at three spiked levels of 10,20 and 100μg/L(orμg/kg)ranged from 92.8%to 117%,with relative standard deviations(RSD)of 0.90%-8.6%.The limit of detection(LOD,S/N≥3)was 5μg/L(orμg/kg),while the limit of quantitation(LOQ,S/N≥10)was 10μg/L(orμg/kg).The method was simple,stable,reliable and sensitive.The food simulants included in the method basically covered the types specified in the regulations and standards.The LOD and LOQ of the method were lower than the specific migration limit(SML)specified in the regulations and standards.The method could not only meet the needs for determination of neopentyl glycol migration in food contact materials and products,but also provide a reliable technical means for related product supervision and quality control.