高效液相色谱法同时测定食品接触材料中九种抗氧剂的特定总迁移量

Simultaneous determination of total specific migration limit of nine types of antioxidants in food stimulants by high performance liquid chromatography with ultraviolet detector

建立了高效液相色谱（HPLC）法检测五种食品模拟物（10％乙醇、3％乙酸、20％乙醇、50％乙醇和异辛烷）中没食子酸丙酯（Nipa49）、没食子酸辛酯（StabilizerGA-8）、没食子酸十二酯（ProgaUinla）、2，4--（十二烷基硫甲基）～6-甲基苯酚（RC1726）、4，6-二（辛硫甲基）邻甲酚（AO1520）、2，2，-亚甲基二[4-甲基-6-（卜甲基环己基）]苯酚（Ion．OXwsp）、2，2＇-甲亚基双（6-环己基-4-甲基酚）（ZKF）、2，2-亚甲基双-（1，1-二甲基乙基）-4-乙基苯酚（A0425）和2，2。亚甲基双-（4-甲基-6-叔丁基苯酚）（AO2246）九种抗氧剂的特定总迁移量fsML（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）的四氢呋喃1：1稀释，经亲水性聚四氟乙烯针头过滤器过滤后进样；异辛烷食品模拟物旋蒸氮吹浓缩至近干，用含0．05％TCEP的甲醇定容，再经亲水性聚四氟乙烯针头过滤器过滤后进样。用c。柱梯度洗脱分离；检测波长为285nm；进样量为20uL；方法在五种食品模拟物中的定量限为0．005—1．0mr／L；水基食品模拟物在3—72、0．5-12、0．3。7．2或0．15--3.6mg/L，异辛烷食品模拟物在30—720、5～120、3-72或1．5～36mg／L范围内线性关系良好（厶0．9982）；0．3～84mg／L三水平的加标回收率为83．7％～113％，相对标准偏差为0．8％～11．2％。结果表明，该方法色谱分离和线性关系较好，回收率和准确度较高，定量限完全满足欧盟（EU）NO10／201I法规附表2中九种抗氧剂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 （Ni- pa 49（CAS：121-79-9）, Stabilizer GA-8（CAS：1034-01-1）, Progallinla（CAS：l166-52-5）, RC 1726（CAS： 110675-26- 8）, AO 1520（CAS：110553-27-0）, Ionox wsp（CAS：77-62-3）, ZKF（CAS：4066-02-8）, AO 425（CAS：88-24-4）and AO 2246 （CAS： 119-47-1 ） ） in food simulants was developed by high performance liquid chromatography （HPLC） with ul- traviolet detector. After the migration test, the soaking solution was cooled down, and vortexed. Each type of aqueous food stimulant （ 10% ethanol, 3% acetic acide, 20% ethanol or 50% ethanol） was diluted with tetrabydrofuran with 0.05% tris- （2-carboxyethyl）-phosphine hydrochloride （TCEP）, and the fatty food simulant i sooctane was concentrated by 10 times,and then a filtration was performed with a disposable syringe and hydrophilic polytetrafluoroethylene before injection. The SunFireTM C8 column and gradient elution mode were selected; the detector was set at 285 nm. The limits of quantification were between 0.005~1.0 mg/L; the linearity of the method was good with r2〉0.9982 over the concentration range from 30-720, 5-120, 3-72 or 1.5-36 mg/L for isooctane, and 3-72, 0.5-12, 0.3-7.2 or 0.15-3.6 mg/L for aqueous food simulants; The recoveries of nine antioxidants were between 83.7% and 113 % with the relative standard deviation between 0.8% and 11.2% at the level range of 0.3-84mg/L. The method shows the lower limits of quantifacations, good recoveries and accuracies, and met the requirement of （EU）NO 10/2011 regulation for the total specific migration limit of nine antioxidants. The method has been applied to analyze food contact material samples.