高效液相色谱-串联质谱法同时测定食品接触材料中间苯二酚-o,o’-二乙酸、2-羟基-6-萘甲酸、间苯二甲酸二甲酯-5-磺酸钠的特定迁移量

Simultaneous determination of specific migration limit of benzene-1,3-dioxyacetic acid,2-hydroxy-6-naphthoic acid and dimethyl 5-sulfoisophthalate sodium salt in food stimulants by high performance liquid chromatography-tandem mass spectrometry

建立了高效液相色谱-串联质谱（HPLC-MS／MS）法同时测定食品模拟物（10％乙醇、3％乙酸、20％乙醇、50％乙醇和橄榄油）中间苯二酚-O，O’-二乙酸、2-羟基-6-萘甲酸、间苯二甲酸二甲酯-5-磺酸钠的特定迁移量（SM）。水基食品模拟物样品经亲水性聚四氟乙烯针式过滤器过滤后进样；橄榄油食品模拟物样品用0．1％乙酸铵溶液震荡提取12min后，静置15min，下清液用亲水性聚四氟乙烯针式过滤器过滤后进样。用C8柱梯度洗脱分离；Qtrap4500质谱在电喷雾离子源负离子及多反应监测（MRM）模式下进行检测。方法在5种食品模拟物中的定量限为0．3-1．2μg／kg；水基食品模拟物在10～200μg／L、橄榄油食品模拟物在10～200μg／kg范围内线性关系良好（r〉0．99904）；加标回收率为86．0％～116％，相对标准偏差为0．5％～7．2％。方法满足欧盟（EU）NO10／2011法规附表l中间苯二酚-O，O’-二乙酸、2-羟基-6-萘甲酸、间苯二甲酸二甲酯-5-磺酸钠的SM限量要求。方法已应用于实际样品的检测。

A novel method for simultaneous determination of specific migration （SM） of benzene-1,3-dioxyacetic acid, 2-hydroxy-6-naphthoic acid and dimethyl 5-sulfoisophthalate sodium salt in food simulants （ 10% ethanol,3% acetic acid, 20% ethanol, 50% ethanol and olive oil） was developed using high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS）. After the migration test, the soaking solution was cooled down, and vortexed. After the extraction of olive oil food simulants with 0. 1% ammonium acetate aqueous solution and n-heptane, the clear aqueous solution or other aqueous food simulants was filtered through a hydrophilic polytetrafluoroethylene filter with a disposable syringe before injection. The SunFire Cs column and gradient elution mode were selected. The AB Qtrap 4500 tandem quadrupole mass spectrometer was operated in multiple reaction monitoring （MRM） and ESI-mode. The limits of quantification were between 0.3 - 1.2 μg/kg; the linearity of the method was good with r 〉 0. 999 over the concentration range from 10. 0 to 200 μg/L or 10.0 to 200μg/kg. The recoveries of them were between 86.0% and 116% with the relative standard deviations between 0. 5% and 7.2% at the level of 20. 0, 50. 0 and 160 mg/kg. The method shows the lower limits of quantification, good recoveries and precisions, and met the requirement of （EU） NO 10/2011 regulation for the specific migration limit of benzene-l, 3-dioxyacetic acid, 2-hydroxy-6-naphthoic acid and dimethyl 5-sulfoisophthalate sodium salt. The method has been applied to analyze food contact material samples.