高效液相色谱-串联质谱法同时检测食品接触材料中9种抗氧剂的特定总迁移量

Simultaneous determination of total speific migration limit of nine antioxidants in food simulants by high performance liquid chromatography-tandem mass speetrometry

建立了高效液相色谱-串联质谱（HPLC-MS/MS）联用方法同时测定塑料制品食品模拟物（10%乙醇、20%乙醇、50%乙醇、3%乙酸和橄榄油）浸泡液中9种抗氧剂的特定总迁移量[SML（T）]。食品模拟物浸泡待测样品,冷却至室温并混匀,水基食品模拟物（10%乙醇、3%乙酸、20%乙醇、50%乙醇）用含0.05%三（2-羧乙基）膦盐酸盐（TCEP）60%的四氢呋喃水基食品模拟物溶液稀释5倍后,经亲水性聚四氟乙烯针头过滤器过滤后进样;橄榄油用甲醇正庚烷提取后,下清液用亲水性聚四氟乙烯针头过滤器过滤后进样。用C8柱梯度洗脱分离;质谱具电喷雾离子源,在负离子多反应监测（MRM）模式下运行;方法在5种食品模拟物中的定量限为0.01～0.3 mg/kg;水基食品模拟物在0.03～0.72 mg/L,0.06～1.44 mg/L,0.1～2.4 mg/L或0.3～7.2 mg/L,橄榄油食品模拟物在0.15～3.6 mg/kg,0.3～7.2 mg/kg,0.5～12.0 mg/kg或1.5～36 mg/kg范围内线性关系良好（R≥0.99240）;0.3～21 mg/kg水平的加标回收率为74.4%～132%,相对标准偏差为0.8%～20%。方法满足欧盟（EU）NO 10/2011法规附表2中9种抗氧剂SML（T）的限量要求,并已应用于实际样品的检测。

A novel method for simultaneous determination of total specific migration limits （SML （T）） of 9 antioxidants in food simulants was developed by 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 from food simulant with methanol and n-heptane, the clear methanol solution and other aqueous food stimulant diluted with aqueous food simulant with 0.05% TCEP and 60% tetrahydrofuran by 5 times were filtered through a hydrophilic polytetrafluoroethylene filter with a disposable syringe before injection. The Cs column and gradient elution mode were selected. The limits of quantification were between 0.01 ～ 0.3 mg/kg; the linearity of the method was good with r ≥ 0. 99240 over the concentration range from 0.03 ～ 0.72 mg/L, 0.06 ～ 1.44 mg/L, 0. 1 -2.4 mg/L or 0.3 ～ 7.2 mg/L for aqueous food simulants,and 0.15 ～ 3.6 mg/kg, 0. 3 -7.2 mg/L,0. 5 - 12. 0 mg/L or 1.5 - 36 mg/kg for olive oil food simulants. The recoveries of nine antioxidants were between 74. 4% and 132% with the relative standard deviation between 0. 8% and 20% at the level range of 0. 3 -21 mg/kg. The method met the requirement of （EU）NO i0/2011 regulation for the total specific migration limit of nine antioxidants. The method has been applied to analyze food contact material samples.