植物油中3种抗氧化剂的同时快速分析

建立了向量–子空间夹角判据结合紫外分光光度法测定植物油中3种抗氧化剂的方法,可用于植物油中特丁基对苯二酚(TBHQ)、丁基羟基茴香醚(BHA)、二丁基羟基甲苯(BHT)3种抗氧化剂的同时快速分析。采用紫外光谱–高效液相色谱(UV-HPLC)联用方法对植物油样品进行分离,构建不含待测组分的本底光谱数据库,基于向量-子空间夹角判据算法的步骤分析植物油中3种抗氧化剂的含量。实际样品加标回收率在95.2%~103.3%之间,RSD小于3%(n=6)。对市售15种植物油样品进行分析,其中12种植物油样品检出TBHQ,含量为21.34~30.12μg/m L,15种植物油样品均未检出BHA和BHT。方法适用于植物油中TBHQ,BHA和BHT 3种抗氧化剂的同时快速分析。     

固相萃取–气相色谱–串联质谱法测定塑料食品包装材料中3种抗氧化剂的残留量

建立了气相色谱–串联质谱法测定塑料食品包装材料中抗氧化剂二丁基羟基甲苯(BHT)、丁基羟基茴香醚(BHA)和特丁基对苯二酚(TBHQ)残留量的分析方法。样品采用环己烷–乙酸乙酯混合溶剂超声萃取,经固相萃取法富集和净化,采用气相色谱–串联质谱在多反应监测模式下进行测定。结果表明,3种抗氧化剂质量浓度在0.05~20 mg/L范围内线性关系良好,线性相关系数大于0.999;BHT,BHA,TBHQ的检出限分别为0.005,0.01,0.03mg/kg;平均添加回收率为88.7%~104.0%;测定结果的相对标准偏差小于5.5%(n=6)。该方法操作简便,灵敏度高,重复性好,可用于塑料食品包装材料中抗氧化剂BHT,BHA,TBHQ残留量的测定。     

高效液相色谱法测定芝麻油中的叔丁基羟基茴香醚、2,6-二叔丁基对甲酚、特丁基对苯二酚

建立高效液相色谱法测定芝麻油中叔丁基羟基茴香醚(BHA)、2,6-二叔丁基对甲酚(BHT)、特丁基对苯二酚(TBHQ)的含量。用25 mL甲醇分5次涡旋超声提取芝麻油中的BHA,BHT,TBHQ,以La Chrom C18(250mm×4.6 mm,5μm)为色谱柱,以甲醇–0.5%甲酸水溶液为流动相进行梯度洗脱,流量为1.0 mL/min,进样体积为5μL,柱温为35℃,检测波长为280 nm。BHA,BHT,TBHQ的质量浓度在20～300 mg/L范围内与其色谱峰面积呈良好的线性关系,相关系数大于0.999,方法检出限为0.5～1.0 mg/kg。样品加标回收率为95.1%～99.8%,测定结果的相对标准偏差为2.1%～4.7%(n=6)。该方法操作简单,试剂用量少,准确度高,精密度好,适用于芝麻油中BHA,BHT,TBHQ含量的日常检测。     

气相色谱法测定高分子食品包装材料中抗氧化剂的残留量

建立了气相色谱测定高分子食品包装材料中抗氧化剂丁基羟基茴香醚(BHA)、二丁基羟基甲苯(BHT)和特丁基对苯二酚(TBHQ)残留量的分析方法。用环己烷超声萃取高分子食品包装材料样品,考察了萃取时间、温度对抗氧化剂萃取量的影响。萃取液经气相色谱柱HP-50+毛细管柱(30 m×0.53 mm×1 μm)分离,电子捕获检测器(ECD)检测,外标法定量。结果表明: 在抗氧化剂添加量为3.00～10.0 mg/kg范围内,BHT、BHA、TBHQ在高分子食品包装材料中的平均添加回收率分别为88%～93%、92%～101%和83%～97%,相对标准偏差(RSD, n=5)分别为2.01%～2.89%、2.11%～3.19%和2.99%～4.02%;检出限(信噪比为3)分别为0.5、0.5和0.8 mg/kg。对实际高分子食品包装材料样品的检测结果表明3种抗氧化剂在不同材质中均有检出: 塑料材料中抗氧化剂的含量较少,仅有BHT、BHA被检出,含量为6.3～7.8 mg/kg;橡胶材料中3种抗氧化剂均被检出,含量为9.3～28.4 mg/kg。该方法准确、灵敏、重现性好,适用于高分子食品包装材料中抗氧化剂残留量的检测。     

气相色谱-质谱法同时测定食用植物油中三种抗氧化剂

本文研究了用乙醇提取食用植物油中的丁基羟基茴香醚(BHA)、二丁基羟基甲苯(BHT)和叔丁基对苯二酚(TBHQ),并用气相色谱-质谱法对三种抗氧化剂进行分离与测定。方法的线性范围为0.100~20.0 mg/L,检出限为:BHA,3.33μg/L;BHT,3.02μg/L;TBHQ,37.9μg/L。平均回收率为80.6%~123%,相对标准偏差为2.01%~8.77%。该方法具有简便、快速、准确、无毒等特点,应用于大豆油、花生油、芝麻油、菜籽油、茶油、食用调和油中的抗氧化剂的测定,结果令人满意。     

固相萃取-高效液相法测定炒货食品及坚果制品中的多种抗氧化剂

运用固相萃取和高效液相色谱技术,建立炒货食品及坚果制品中丁基羟基茴香醚(BHA)、二丁基羟基甲苯(BHT)、叔丁基对苯二酚(TBHQ)、没食子酸丙酯(PG)等人工合成的抗氧化剂和茶多酚、甘草抗氧化物、迷迭香提取物等天然抗氧化剂的测定方法。样品经甲醇、异丙醇、乙腈等混合溶剂提取,冷冻离心后经C18柱固相萃取净化,用高效液相色谱检测。各抗氧化剂残留量在6~100 mg/L范围内呈良好线性关系,加标回收率为80%~106%。     

气相-质谱选择离子法测定化妆品中抗氧化剂丁基羟基茴香醚、二丁基羟基甲苯

 采用气相 质谱 (选择离子方式 )测定化妆品中抗氧化剂丁基羟基茴香醚 (BHA)和二丁基羟基甲苯(BHT) ,样品用甲醇振荡萃取 ,以SupelcoWAXTM 10 (30m× 0 2 5mmi.d .× 0 2 5 μm)为分析柱。该方法对样品中BHA和BHT的检测限分别为 2 5 μg/g和 0 5 μg/g。方法简便、快速、灵敏 ,可用于多种化妆品的检验。     

反相高效液相色谱-荧光法同时测定食品中叔丁基对苯二酚和叔丁基羟基茴香醚的含量

1 引言 油溶性抗氧化剂叔丁基对苯二酚(tert-butyl hydroquinone,TBHQ)、叔丁基羟基茴香醚(butylated hydroxyanisole,BHA)和2,6-二叔丁基对甲酚(butylated hydroxytoluene,BHT)是目前最常用的化学合成抗氧化剂,能够有效阻止或延迟油脂氧化变质.     

高效液相色谱法测定油脂中抗氧化剂BHA、TBHQ

采用乙腈浸提油脂中抗氧化剂叔丁基羟基茴香醚(BHA)和特丁基对苯二酚(TBHQ)，用以乙腈-水淋洗的反相高效液相色谱法测定提取液中BHA，TBHQ，回收率为92.42％～96．69％，变异系数为2．26％～2．88％，方法简便、快速、准确，已用于油脂中抗氧化剂BHA、TBHQ的测定。     

高效液相色谱法同时测定食用油脂和膨化食品中的3种抗氧化剂

建立同时测定食用油脂和膨化食品中3种抗氧化剂丁基羟基茴香醚(BHA)、二丁基羟基甲苯(BHT)、特丁基对苯二酚(TBHQ)的高效液相色谱法.样品经甲醇提取后,以甲醇-0.1%甲酸溶液为流动相梯度洗脱,C18色谱柱分离,采用高效液相色谱法(HPLC)-二极管阵列检测器(DAD),在检测波长280 nm,参比波长360 n...     

Determination of synthetic phenolic antioxidants in essence perfume by high performance liquid chromatography with vortex-assisted,cloud-point extraction using AEO-9

This study aimed to establish a rapid analytical method to determine antioxidants in essence. A simple,efficient and practical, vortex-assisted, cloud-point extraction(VACPE) procedure is proposed for extracting and pre-concentrating four different of synthetic phenolic antioxidants(SPAs), propyl gallate(PG), tert-butylhydroquinone(TBHQ), butylated hydroxyanisole(BHA), butylated hydroxytoluene(BHT) in essence prior to high performance liquid chromatography(HPLC) analysis. The non-ionic surfactant, fatty alcohol polyoxyethylene ether-9(AEO-9), was used as extractant and vortex-mixing was utilized to reduce extraction time and improve extraction efficiency. The effective parameters of the extraction process, such as volume of extraction solvent, pH, vortex-mixing time, equilibration temperature and time, were optimized. Under the optimum conditions, the linear range of PG, TBHQ,BHA and BHT was 8.0–800 ng/mL. All correlation coefficients of the calibration curves were higher than0.996 and relative standard deviations(RSD, n = 5) were 2.36%–5.46%. The proposed method was successfully applied to the extraction and determination of antioxidants in essence samples with satisfactory relative recoveries of 89.4%–103.5%. The results confirmed the SPAs of essence could be effectively monitored by this method and also established good reference criteria for essence.     

Glassy carbon electrodes modified with gold nanoparticles for the simultaneous determination of three food antioxidants

Electrochemical behavior of three antioxidants: butylated hydroxyanisole (BHA), butylated hydroxytoluene (BHT) and butylated hydroquinone (TBHQ), was investigated at a glassy carbon electrode modified with gold nanoparticles (AuNPs/GCE). This electrode was characterized by scanning electron microscopy (SEM). The experimental results indicated that the modified electrode was strongly electroactive during the redox reactions of BHA, BHT and TBHQ, and this was confirmed by the observed increased redox peak currents and shifted potentials; in addition, the oxidation products of BHA and TBHQ were found to be the same. The experimental conditions were optimized and the oxidation peaks of BHA and BHT were clearly separated. Based on this, an electrochemical method was researched and developed for the simultaneous determination of BHA, BHT and TBHQ in mixtures with the use of first derivative voltammetry; the linear concentration ranges were 0.10–1.50 μg mL⁻¹, 0.20–2.20 μg mL⁻¹ and 0.20–2.80 μg mL⁻¹, and detection limits were 0.039, 0.080 and 0.079 μg mL⁻¹, for BHA, BHT and TBHQ, respectively. The proposed method was successfully applied for the analysis of the three analytes in edible oil samples.     

Determination of antioxidants in cosmetics by micellar electrokinetic capillary chromatography with electrochemical detection

A new and efficient method for the determination of antioxidants [Propyl gallate (PG), tert-butylhydroquinone (TBHQ), butylated hydroxyanisole (BHA), and butylated hydroxytoluene (BHT)] in cosmetics has been established by using micellar electrokinetic capillary chromatography with electrochemical detection (MECC-ED). Under the optimum conditions of the method, all analytes were successfully separated within 13 min at the separation voltage of 18 kV in a 20 mmol/L borate running buffer (pH 7.4) containing 25 mmol/L sodium dodecyl sulfate. The excellent linearity was obtained in the concentration range from 5.0 x 10(-4) to 2.0 x 10(-6) mol/L and the detection limits (S/N = 3) of PG, TBHQ, BHA, and BHT range from 3 x 10(-7) to 3 x 10(-6) mol/L.     

高效液相色谱法测定食品中抗氧化剂BHA,BHT,PG

 用反相高效液相色谱法同时测定了食品中抗氧化剂丁基羟基茴香醚（ＢＨＡ）、二丁基羟基甲苯（ＢＨＴ）和焦性没食子酸丙酯（ＰＧ）。样品用正己烷提取，氮气吹干，水－乙醇（１４，Ｖ／Ｖ）溶解残留物，经０．５μｍ滤膜过滤，直接进样。方法简便、快速、回收率高、重现性好。     

Determination of Phenolic Anti-Oxidants in Edible Oil by High-Performance Liquid Chromatography with Amperometric Detector

Abstract

A high-performance liquid chromatography (HPLC) with amperometric detection was investigated for the analysis of 2-and 3-tert-butyl-4-hydroxyanisole (BHA), 3,5-di-tert?butyl-4-hydroxytoluene (BHT), and tert?butyl-hydroquinone (TBHQ) in edible oil. The reversed-phase system developed was combined with an amperometric detector, the working electrode of which was made of glassy carbon, in order to compare the sensitivity and selectivity of ultraviolet and fluorometric detection. For the amperometric detection of HPLC, cyclic voltammetry was used to monitor the electrochemical properties of the phenolic antioxidants. A simple isolation procedure, based on the continuous liquid-liquid partition technique, was examined for the extraction and clean up of the antioxidants from edible oil. The recovery rates of BHA, BHT, and TBHQ added salad oil were between 90.2-107.7% in the range of 1-50 ppm of the antioxidants. By the present method, BHA, BHT, and TBHQ were well separated, identified and quantitated with a high sensitivity.     

Optimization of a high-performance liquid chromatography system by artificial neural networks for separation and determination of antioxidants

A high-performance liquid chromatography (HPLC) system was used to determine the antioxidants tert-butyl-hydroquinone (TBHQ), tert-butylhydroxyanisole (BHA), and 3,5-di-tert-butylhydroxytoluene (BHT) simultaneously in oils. The paper presents a new methodology for the optimized separation of antioxidants in oils based on the coupling of experimental design and artificial neural networks. The orthogonal design and the artificial neural networks with extended delta-bar-delta (EDBD) learning algorithm were employed to design the experiments and optimize the variables. The response function (Rf) used was a weighted linear combination of two variables related to separation efficiency and retention time, according to which the optimized conditions were obtained. The above-mentioned antioxidants in rapeseed oils were separated and determined simultaneously under optimized conditions by HPLC with UV detection at 280 nm. Linearity was obtained over the range of 10-200 microg/mL with recoveries of 98.3% (TBHQ), 98.1% (BHT), and 96.2% (BHA).     

Separation and Determination of Phenolic Antioxidants by HPLC with Surfactant/n‐Propanol Mobile Phases

The influence of cationic and anionic surfactants and short‐chain alcohols in the mobile phase on the retention of five antioxidants has been studied. The solutes chosen were butylated hydroxyanisole (BHA), butylated hydroxytoluene (BHT), and propyl, octyl, and dodecyl gallates (PG, OG, DG).The surfactants were hexadecyltrimethylammonium bromide (CTAB) and sodium dodecyl sulfate (SDS), and n‐propanol (PrOH) was the selected alcohol. A simple isocratic reversed‐phase method for the antioxidant determination is proposed. Separation of five primary antioxidants takes 18 min with the mobile phase SDS 0.10 M/H₃PO₄ 0.01 M/PrOH 30%. Variation of the percentage of alcohol in the mobile phase permits optimization of the retention times of the antioxidants. Detection limits in the pg range were obtained for the all solutes. The method was used to determine the antioxidants in olive oil at three different levels, giving mean recoveries close to 100% for all the solutes (BHA 102%, PG 99%, OG 99%, DG 99%) except BHT (84%).