甲醇萃取法在食用油中酚类抗氧化剂检测中的应用研究

目的对比国标方法与甲醇萃取法萃取食用油中的酚类抗氧化剂。方法分别用乙酸乙酯:环己烷(1:1,V:V)萃取凝胶渗透色谱仪(gelpermeationchromatograph,GPC)进行样品净化气相色谱检测和甲醇萃取冷冻过滤气相色谱检测。结果甲醇萃取法在检测叔丁基羟基茴香醚(butyl hydroxyl acids, BHA)、2, 6-二叔丁基-4-甲基苯酚(butylated hydroxytoluene, BHT)、叔丁基对苯二酚(tertiary butylhydroquinone, TBHQ) 3种抗氧化剂在各自的线性范围内,线性关系良好,相关系数r大于0.999,相对标准偏差(relative standard deviation RSD)为0.91%～1.75%,回收率为89%～98%。结论该方法简单、快速、准确、实验成本低,适用于食用油中酚类抗氧化剂的测定。     

肉制品中合成抗氧化剂含量的高效液相色谱法测定

建立用高效液相色谱法同时测定肉制品中的合成抗氧化剂叔丁基羟基茴香醚(BHA)、2,6-二叔丁基对甲酚(BHT)、叔丁基对苯二酚(TBHQ)、没食子酸丙酯(PG)含量的方法.将试样中的抗氧化剂用甲醇提取,经0.5μm滤膜过滤,进行色谱分析.方法栓出限BHA为5 mg/kg,BHT、TBHQ、PC为2 mg/kg.3个不同加标水平样品中4个目标化合物的回收率为85%～101%,RSD为3.6%～6.1%(n=6).该方法前处理方法快速、简单,检测结果准确.实现了用高效液相色谱对肉制品中合成抗氧化剂的定量分析.     

PSE-HPLC 法测定食品中叔丁基羟基茴香醚和2,6- 二叔丁基羟基甲苯

目的：建立测定食品中抗氧化剂叔丁基羟基茴香醚(BHA)和2,6- 二叔丁基羟基甲苯(BHT)加压溶剂萃取-高效液相色谱法(PSE-HPLC 法)。方法：采用正交试验对影响PSE 萃取效率的温度、压力、萃取溶剂、萃取时间进行优化,联合HPLC 进行测定,并确定分别以BHA 提取量、BHT 提取量以及总量为评价指标的最优条件。结果：PSE-HPLC 法测定BHT 和BHA 的相对标准偏差(RSD)为0.5%～3.1%,并且在1.0～200.0μg/mL 范围内色谱峰面积与组分质量浓度均有很好的线性相关性(r ≥ 0.9997),检出限为0.05μg/mL,在最优条件下的回收率为92.60%～97.80%。结论：PSE-HPLC 法简便、快速、效率高,方法的重现性、线性相关性以及检出限理想,适用于食品中BHT 和BHA 含量及两者总量的同时快速检测。     

气相色谱法测定菜籽油中BHA和BHT的前处理方法的改进

探讨在测定菜籽油中的叔丁基羟基茴香醚(BHA)和2,6-二叔丁基对甲酚(BHT)等抗氧化剂时,用毛细管色谱柱替换填充柱的效果,以及三种不同的前处理方法对测定结果的影响.结果表明:用乙腈提取或甲醇提取法进行前处理,使用毛细管色谱柱分离的方法可以在较短时间完成BHA和BHT测定,并且线性良好,回收率在90%以上.     

气相色谱--质谱法测定XO酱中BHA、BHT和TBHQ

采用气相色谱—质谱(全扫描方式)测定XO酱中丁基羟基茴香醚(BHA)、二丁基羟基甲苯(BHT)和叔丁基对苯二酚(TBHQ)。样品用甲醇振荡萃取，以DB—5MS为分析柱。3种组分的回收率在85％～99％之间，相对标准偏差小于8．4％；样品中BHA、BHT和TBHQ的检测限分别为0．05、0．05和0．10(mg／kg)。该法简单、快速、准确，可用于XO酱等基质复杂的富油食品中BHA、BHT和TBHQ的检测和确证。     

固相萃取-高效液相色谱法测定水产品中的甲基睾酮残留量

建立水产品中甲基睾酮残留量的固相萃取-高效液相色谱测定方法。样品经乙醚振荡提取、蒸发浓缩、正己烷除脂、LC-C18柱净化后吹干定容,以甲醇-0.1%甲酸溶液(75:25,V/V)为流动相经反相高效液相色谱检测定量。方法在7.0～200μg/kg添加范围内的平均回收率为82.0%～86.0%,相对标准偏差均小于7%,定量限为7.0μg/kg。     

高效液相色谱法测定羽绒制品中烷基酚聚氧乙烯醚

探讨高效液相色谱测定羽绒制品中烷基酚聚氧乙烯醚(APEO)含量的方法。以V(甲醇)∶V(水)=2∶1为萃取剂,在60℃温度下振荡萃取样品1h,以V(甲醇)∶V(水)∶V(乙腈)=80∶15∶5为流动相采用高效液相色谱-二极管阵列检测器对APEO进行分析。实验结果表明:该方法简单快捷、定量准确、重复性好,加标回收率在86.35%~107.07%,相对标准偏差小于6.29%。     

油脂中TBHQ、PG、OG、BHA和BHT的同时检测研究

研究了高效液相色谱同时测定油脂中特丁基对苯二酚(TBHQ)、没食子酸丙酯(PG)、没食子酸辛酯(OG)、叔丁基羟基茴香醚(BHA)和2,6-二叔丁基对甲酚(BHT)的方法。检测波长,280nm;流动相采用甲醇和1%乙酸溶液梯度洗脱;柱温:35℃;流速:1.0mL/min;进样量:5μL。5种组份的回收率在90.7%～102.0%之间,相对标准偏差(RSD)2.50%。     

UPLC测定食用油中10种抗氧化剂

建立超高效液相色谱法同时测定食用油中没食子酸丙酯(PG)、2,4,5-三羟基苯丁酮(THBP)、叔丁基对苯二酚(TBHQ)、没食子酸异戊酯(IAG)、去甲二氢愈创木酸(NDGA)、叔丁基对羟基茴香醚(BHA)、2,6-二叔丁基-4-羟甲基苯酚(Lonox-100)、没食子酸辛酯(OG)、2,6-二叔丁基对甲基苯酚(BHT)、没食子酸十二酯(DG)10种抗氧化剂的方法。样品用乙腈饱和的正己烷溶解,正己烷饱和的乙腈萃取其中的抗氧化剂后,经C18柱分离,甲醇-1%乙酸溶液体系为流动相进行梯度洗脱,紫外检测波长280 nm处检测,外标法定量。结果表明:10种抗氧化剂在1~500mg/L的范围内线性关系良好,r为0.998 7~0.999 6,测定低限不大于1.0 mg/kg;回收率为89.31%~100.20%,RSD在1.98%~5.78%之间。该方法准确、重复性好、灵敏度高,适合食用油中多种抗氧化剂的同时快速测定。     

高效液相色谱法测定15种蔬菜中的β-胡萝卜素

应用高效液相色谱法测定国内常用的15种蔬菜中β-胡萝卜素含量。蔬菜中的β-胡萝卜素经超声提取,用Kromasil C18(4.6mm×300mm,5μm)色谱柱,甲醇-四氢呋喃(THF)-2,6-二叔丁基-4-甲基苯酚(BHT)(9:1:0.01,V/V)为流动相,紫外检测器检测,检测波长为4 4 8 n m。结果表明,β-胡萝卜素出峰时间短(21 m in),检出限低(0.075μg/mL),在1～50μg/mL质量浓度范围内线性关系良好(R2=0.9997),平均加标回收率达97.84%(n=5)。该方法可避免β-胡萝卜素在预处理过程中被氧化,重复性好、操作简便、结果可靠,可用于多种新鲜蔬菜中β-胡萝卜素含量的测定。     

Levels of synthetic antioxidants (ethoxyquin,butylated hydroxytoluene and butylated hydroxyanisole) in fish feed and commercially farmed fish

Several synthetic antioxidants are authorized for use as feed additives in the European Union. Ethoxyquin (EQ) and butylated hydroxytoluene (BHT) are generally added to fish meal and fish oil, respectively, to limit lipid oxidation. The study was conducted to examine the concentrations of EQ, BHT and butylated hydroxyanisole (BHA) in several commercially important species of farmed fish, namely Atlantic salmon, halibut and cod and rainbow trout, as well as concentrations in fish feed. The highest levels of BHT, EQ and BHA were found in farmed Atlantic salmon fillets, and were 7.60, 0.17 and 0.07?mg?kg^?1, respectively. The lowest concentrations of the synthetic antioxidants found were in cod. The concentration of the oxidation product ethoxyquin dimer (EQDM) was more than ten-fold higher than the concentration of parent EQ in Atlantic salmon halibut and rainbow trout, whereas this dimer was not detected in cod fillets. The theoretical consumer exposure to the synthetic antioxidants EQ, BHA and BHT from the consumption of farmed fish was calculated. The contribution of EQ from a single portion (300?g) of skinned fillets of the different species of farmed fish would contribute at most 15% of the acceptable daily intake (ADI) for a 60?kg adult. The consumption of farmed fish would not contribute measurably to the intake of BHA; however, a 300?g portion of farmed Atlantic salmon would contribute up to 75% of the ADI for BHT.     

Determination of synthetic phenolic antioxidants in soft drinks by stir-bar sorptive extraction coupled to gas chromatography-mass spectrometry

The synthetic phenolic antioxidants butylated hydroxyanisole (BHA), butylated hydroxytoluene (BHT) and tert-butyl hydroquinone (TBHQ) were pre-concentrated by stir-bar sorptive extraction and thermally desorbed (SBSE-TD) before analysis by GC-MS. Several parameters affecting the derivatisation step and both SBSE extraction and thermal desorption were carefully optimised. When the analyses of BHA and TBHQ in their acetylated, silylated and underivatised forms were compared, the best results were obtained when the in-situ derivatisation procedure with acetic anhydride was employed. Quantification was carried out using carvacrol as the internal standard, providing quantification limits of between 0.11 and 0.15 ng ml^?1, depending on the compound. Recovery assays for samples spiked at two concentration levels, 1 and 5 ng ml^?1, provided recoveries in the 81–117% range. The proposed method was applied in the analysis canned soft drinks and the analytes were found in five of the 10 samples analysed.     

Gas Chromatographic Determination of Butylated Hydroxyanisole, Butylated Hydroxytoluene and Tertiarybutyl Hydroquinone in Soybean Oil

Oils containing different levels of the most common phenolic antioxidants, butylated hydroxyanisole (BHA), butylated hydroxytoluene (BHT), and tertiarybutyl hydroquinone (TBHQ) from 0–200 ppm were analyzed by a new gas chromatographic method. The antioxidants in oils were isolated by nitrogen gas purging, collected on Tenax GC coated with polymetaphenoxylene, and then separated and quantitated by gas chromatography. This method requires neither extraction of antioxidants from oil nor derivatization of antioxidants. The correlation coefficients (r) between gas chromatographic peak heights or peak area and their concentrations in oils were 0.99 for BHA, BHT, and TBHQ. This simple gas chromatographic method can determine as little as 10 ppm pf BHA, BHT, or TBHQ in oils in an hour.     

气相色谱法测定食用油中BHA和BHT残留量的对比研究

目的建立气相色谱法测定食用油中叔丁基羟基茴香醚(butyl hydroxyanisole,BHA)和二丁基羟基甲苯(butylated hydroxytoluene,BHT)的残留量。方法使用无水乙醇萃取样品,经中性氧化铝吸附杂质,HP-5毛细管柱分离,使用气相色谱仪定量分析BHA和BHT在食用油中的残留量。同时,与GB/T 5009.30中的方法进行对比,考察了本方法的线性、重现性、回收率和精密度。结果本方法中BHA和BHT的线性范围分别为2.02~40.48 ng和2.07~41.36 ng,标准曲线方程分别为Y=16.61X+10.03(r=0.9996)和Y=20.14X+16.56(r=0.9997);BHA和BHT的检出限分别为92.4 ng/kg和108.6 ng/kg,加标回收率分别为98.94%(相对标准偏差为0.33%)、98.69%(相对标准偏差为0.34%)。结论本实验建立的方法灵敏度高、定量准确,和国标法相比,具有简单实用的特点,适合食用油中BHA和BHT残留量的检测。     

QuEChERS-高效液相色谱法快速检测食用油中4种抗氧化剂

目的 建立QuEChERS-高效液相色谱法(high performance liquid chromatography, HPLC)快速测定食用油中没食子酸丙酯(propyl gallate, PG), 特丁基对苯二酚(tertiary butylhydroquinone, TBHQ), 叔丁基对羟基茴香醚(butyl hydroxyanisd, BHA), 2,6-二叔丁基对甲酚(butylated hydroxytoluene, BHT)4种抗氧化剂的分析方法。方法 样品用乙腈提取, 经C18-无水MgSO4粉末净化, 色谱柱分离, 以0.5%甲酸水溶液和甲醇为流动相进行梯度洗脱, 二极管阵列检测器(diode array detector, DAD)检测, 检测波长280 nm。结合保留时间和紫外光谱进行定性分析, 峰面积进行定量分析。结果 4种抗氧化剂质量浓度在2.0~100 mg/L范围内线性良好, 相关系数r2＞0.9994; 在不同种类食用油中3个添加水平的平均回收率为78.8%~94.5%, 相对标准偏差为1.1%~6.8%。结论 该方法简便、快捷、节约溶剂, 适用于食用油中快速检测4种抗氧化剂。     

Cloud-point extraction and reversed-phase high-performance liquid chromatography for the determination of synthetic phenolic antioxidants in edible oils

A cloud-point extraction (CPE) method using Triton X-114 (TX-114) nonionic surfactant was developed for the extraction and preconcentration of propyl gallate (PG), tertiary butyl hydroquinone (TBHQ), butylated hydroxyanisole (BHA), and butylated hydroxytoluene (BHT) from edible oils. The optimum conditions of CPE were 2.5% (v/v) TX-114, 0.5% (w/v) NaCl and 40 min equilibration time at 50 °C. The surfactant-rich phase was then analyzed by reversed-phase high-performance liquid chromatography with ultraviolet detection at 280 nm, using a gradient mobile phase consisting of methanol and 1.5% (v/v) acetic acid. Under the studied conditions, 4 synthetic phenolic antioxidants (SPAs) were successfully separated within 24 min. The limits of detection (LOD) were 1.9 ng mL(-1) for PG, 11 ng mL(-1) for TBHQ, 2.3 ng mL(-1) for BHA, and 5.9 ng mL(-1) for BHT. Recoveries of the SPAs spiked into edible oil were in the range 81% to 88%. The CPE method was shown to be potentially useful for the preconcentration of the target analytes, with a preconcentration factor of 14. Moreover, the method is simple, has high sensitivity, consumes much less solvent than traditional methods, and is environment-friendly. Practical Application: The method established in this article uses less organic solvent to extract SPAs from edible oils; it is simple, highly sensitive and results in no pollution to the environment.     

Evaluation of food grade antioxidant formulation for sustained antifungal,antiaflatoxigenic and insecticidal activities on peanut conditioned at different water activities

The aim of this study was to investigate antifungal and insecticidal activity of two microencapsulated antioxidants: 2(3)-tert-butyl-4 hydroxyanisole (BHA) and 2,6-di(tert-butyl)-p-cresol (BHT) against Aspergillus section Flavi and Oryzaephilus surinamensis (L.), a vector carrier of aflatoxigenic fungi on stored peanuts. Susceptibility of Aspergillus section Flavi, insects, and aflatoxin B₁ accumulation in sterile peanut kernels conditioned at two different water activities (a_w) (0.83 a_w and 0.95 a_w) was determined with different doses of antioxidant formulations (10, 20 and 30 mM) during 45 days. Moreover, Aspergillus section Flavi isolation frequency from live and dead insects was evaluated. The BHA formulation completely inhibited Aspergillus section Flavi development regardless of a_w and doses assayed. Antifungal effect of microencapsulated BHT was highly dependent on a_w, with 86–100% fungal inhibition at 20 and 30 mM, at the lowest a_w (0.83 a_w) and at the end of the experiment. No aflatoxin accumulation was detected in samples treated with the BHA formulation. In general, low levels of Aspergillus section Flavi were detected in dead insects. Our results show efficacy for 45 days, in addition microencapsulated BHT could be an alternative to control peanut pests in dry kernels.     

Analysis of synthetic phenolic antioxidants in edible oils by micellar electrokinetic capillary chromatography

Synthetic antioxidants most used in oil-based food to avoid oxidation processes, butylated hydroxyanisole (BHA), butylated hydroxytolueno (BHT), and dodecyl gallate (DG), were analyzed in edible oils using micellar electrokinetic capillary chromatography (MECK) with bis-(2-ethylhexyl) sodium sulfosuccinate as the pseudostationary phase.

Studies involving solid-phase and liquid–liquid extraction were performed to find the best sample treatment before injection into the electrophoretic system. The best methodology for the isolation of antioxidants was extraction with acetonitrile from edible oil diluted with hexane. A method that allows the determination of the antioxidants present in these samples was proposed. With this method BHA, BHT and DG were evaluated at levels permitted in the European Union.