CAJ | 학술논문

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（Nipa 49）、没食子酸辛酯（Stabilizer GA-8）、没食子酸十二酯（Progallinla）、2，4-二（十二烷基硫甲基）-6-甲基苯酚（RC 1726）、4，6-二（辛硫甲基）邻甲酚（AO 1520）、2，2'-亚甲基二[4-甲基-6-（1-甲基环己基）]苯酚（Ion?ox wsp）、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（AO 425）和2，2'-亚甲基双-（4-甲基-6-叔丁基苯酚）（AO 2246）九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）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C8柱梯度洗脱分离；检测波长为285 nm；进样量为20μL；方法在五种食品模拟物中的定量限为0.005~1.0 mg/L；水基食品模拟物在3~72、0.5~12、0.3~7.2或0.15~3.6 mg/L，异辛烷食品模拟物在30~720、5~120、3~72或1.5~36 mg/L范围内线性关系良好（r2>0.9982）；0.3~84 mg/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）NO 10/2011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。
건립료고효액상색보（HPLC）법검측오충식품모의물（10%을순、3%을산、20%을순、50%을순화이신완）중몰식자산병지（Nipa 49）、몰식자산신지（Stabilizer GA-8）、몰식자산십이지（Progallinla）、2，4-이（십이완기류갑기）-6-갑기분분（RC 1726）、4，6-이（신류갑기）린갑분（AO 1520）、2，2'-아갑기이[4-갑기-6-（1-갑기배기기）]분분（Ion?ox wsp）、2，2'-갑아기쌍（6-배기기-4-갑기분）（ZKF）、2，2'-아갑기쌍-（1，1-이갑기을기）-4-을기분분（AO 425）화2，2'-아갑기쌍-（4-갑기-6-숙정기분분）（AO 2246）구충항양제적특정총천이량[SML（T）]。식품모의물침포대측양품，냉각지실온병혼균，수기식품모의물（10%을순、3%을산、20%을순、50%을순）용함0.05%삼（2-최을기）련염산염（TCEP）적사경부남1：1희석，경친수성취사불을희침두과려기과려후진양；이신완식품모의물선증담취농축지근간，용함0.05%TCEP적갑순정용，재경친수성취사불을희침두과려기과려후진양。용C8주제도세탈분리；검측파장위285 nm；진양량위20μL；방법재오충식품모의물중적정량한위0.005~1.0 mg/L；수기식품모의물재3~72、0.5~12、0.3~7.2혹0.15~3.6 mg/L，이신완식품모의물재30~720、5~120、3~72혹1.5~36 mg/L범위내선성관계량호（r2>0.9982）；0.3~84 mg/L삼수평적가표회수솔위83.7%~113%，상대표준편차위0.8%~11.2%。결과표명，해방법색보분리화선성관계교호，회수솔화준학도교고，정량한완전만족구맹（EU）NO 10/2011법규부표2중구충항양제SML（T）적한량요구，병이응용우실제양품적검측。
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:1166-52-5),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 tetrahydrofuran with 0.05%tris-(2-carboxyethyl)-phosphine hydrochloride(TCEP),and the fatty food simulant isooctane was concentrated by 10 times,and then a filtration was performed with a disposable syringe and hydrophilic polytetrafluoroethylene before injection. The SunFire TM 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 to?tal specific migration limit of nine antioxidants. The method has been applied to analyze food contact material samples.