油炸薯条中酚类抗氧化剂的高效液相色谱法测定

采用反相高效液相色谱法测定油炸薯条中PG、TBHQ、BHA、4HR、BHT、2246.其中PG、TBHQ用50%甲醇(体积分数1%的冰醋酸)作流动相,BHA、4HR、BHT、2246用80%的甲醇作流动相,检测波长为280nm,用纯甲醇提取样品中的PG、TBHQ;用甲醇∶二氯甲烷=9∶ 1(V/V)提取BHA、4HR、BHT、2246.相关系数在0.9983～0.9996之间,检出限为1.0～2.0μg/g ,标准偏差在0.21%～5.30%之间,平均回收率均在85%以上.     

油脂及油炸食品中四种抗氧化剂的同时测定

建立采用高效液相色谱仪同时测定油脂及油炸食品中PG、TBHQ、BHA、BHT 4种抗氧化剂的方法.样品的抗氧化剂经甲醇提取、过滤后即可直接测定.流动相为1%乙酸水溶液和甲醇,梯度洗脱,4种组分能有效分离,出峰时间在15 min内,回收率在84.2%～99.2%之间,相对标准偏差RSD<5%.该方法简单、快速、准确,可用于油脂及油炸食品中PG、TBHQ、BHA和BHT的同时检测.     

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%。     

HPLC法测定花生酱中BHA、BHT和TBHQ

采用甲醇浸提花生酱中的抗氧化剂BHA、BHT和TBHQ,浓缩后用甲醇-水淋洗的反相高效液相色谱法测定其中的抗氧化剂含量,检测波长为280nm;流动相甲醇∶水=20∶80;梯度:20%～80%甲醇/5～20min,80%甲醇保持5min。3种抗氧化剂的回收率在85.25%～103.91%,变异系数为2.07%～3.80%,该方法简便、快速、准确,适用于花生酱中BHA、BHT和TBHQ的检测。     

亚麻油中TBHQ、BHA和BHT的同时快速检测

建立了高效液相色谱法同时快速测定亚麻油中特丁基对苯二酚(TBHQ)、叔丁基茴香醚(BHA)和2,6-二叔丁基对甲酚(BHT)3种抗氧化剂的方法。采用甲醇(5 m L+5 m L)直接提取亚麻油中的TBHQ、BHA和BHT,C18柱(4.6 mm×250 mm×5μm)进行分离,紫外检测器检测。流动相用甲醇和1%乙酸梯度洗脱,流速为1.0 m L/min,进样量为10μL,检测波长为280 nm。3种抗氧化剂的检出限:TBHQ为0.04μg/m L,BHA为0.01μg/m L,BHT为0.02μg/m L,回收率为91.2%~103.6%;相对标准偏差在2.5%~6.8%之间。     

气相色谱法同时检测含油脂食品中BHA、BHT和TBHQ的改进

选用含油脂样品,甲醇提取,采用气相色谱法检测食品中的BHA、BHT、TBHQ指标。结果发现,在浓度为0.01～0.20mg/mL时,BHA、BHT与TBHQ均呈现出较好的线性关系,其相关系数r均0.999,检出限均0.5μg/mL;检测方法回收率符合实验室测定要求,其标准偏差为1.07～3.10,相对标准差均5%。     

高效液相色谱法快速测定食品中的四种抗氧化剂

用高效液相色谱法测定油脂食品中丁基羟基茴香醚（BHA）、二丁基羟基甲苯（BHT）特丁基对苯二酚（TBHQ）和没食子酸丙酯（PG）。样品用甲醇均质提取后,经冷却、离心分离去除残留油脂。以乙酸水溶液（pH3．0）/甲醇为流动相,二液梯度洗脱,用250mm×4．6mm C1810μm柱、紫外检测器在波长280nm处测定吸光强度,外标法定量,检出限TBHQ：0．26μg／ml,PG：0．10μg／ml,BHA：0．16μg／ml,BHT：0．16μg／ml;加标回收率93．8％～102．4％。     

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。     

液相色谱法同时快速测定植物油中TBHQ、BHA、BHT探讨

采用NY/T 1602-2008液相色谱条件分析TBHQ、BHA和BHT时,结果发现色谱图基线不稳,有杂峰干扰结果准确定量,导致BHT不能建立良好线性标准工作曲线。为建立同时快速测定该三种抗氧化剂方法,该研究采用甲醇―水(体积比85∶15)进行等梯度洗脱,对比三种标准物质色谱图;结果表明,荧光检测器(FLD)更适于定量检测TBHQ和BHA;紫外检测器(VWD)更适于定量检测BHT;色谱图均基线平稳、峰形良好,无杂峰干扰,TBHQ、BHA和BHT均能建立良好线性标准工作曲线,相关系数分别为0.99999、0.99963和0.99999;TBHQ、BHA和BHT平均加标回收率分别为102.68%、110.97%和102.39%;相对标准偏差分别为3.87%、2.46%和1.98%(n=10)。该法前处理简单、定量快速准确、方法回收率高、精密度好,适于同时快速测定植物油中TBHO、BHA、BHT三种抗氧化剂。     

钛胶RP-HPLC法测定食用油及其制品中的TBHQ、PG和BHT

建立了反相钛胶柱高效液相色谱法同时测定油脂及其制品中特丁基对苯二酚(TBHQ)、没食子酸丙酯(PG)和2,6-二叔丁基对甲酚(BHT)的方法.色谱条件:分离柱为Titania Sachtopore-RP柱(250 mm×4.6 mm i.d.,5μm);流动相采用1.0％的磷酸-甲醇-水梯度洗脱;流速为0.8 mL/min;检测波长为290 nm;TBHQ、PG的线性回归范围为0.5～50 μg/mL;BHT线性回归范围为0.5～ 100 μg/mL;TBHQ、PG和BHT的最低检出限分别为0.2、0.1和2.0 μg/mL;样品的加标回收率范围为91.61％ ～ 114.11％.该方法操作简单易行,方法精密度和准确度高,用于食用油及其制品中TBHQ、PG和BHT的同时测定,取得满意结果.     

Qualitative and Quantitative Effects of Antioxidants on the Flavor Stability of Oil

Qualitative and quantitative effects of the common antioxidants, BHA, BHT, PG and TBHQ on the rate of dissolved free oxygen disappearance in soybean oil during storage were studied. The order of effectiveness was BHA, BHT, PG and TBHQ with TBHQ as the most effective. Statistical analyses of the results showed that the effects of BHA and BHT were not significantly different from each other at the 5% level, but BHA or BHT was different from PG or TBHQ, and PG was different from TBHQ. The antioxidant effectiveness of levels of 0, 50, 100, 150 and 200 ppm BHA, BHT, PG or TBHQ was significantly different from one another at the 5% level. The higher the amounts of antioxidants added, the slower the rate of dissolved oxygen disappearance in the oil.     

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.     

Determination of synthetic phenolic antioxidants in food items using reversed-phase HPLC

A HPLC with gradient elution method for the determination of the synthetic phenolic antioxidants (SPAs) propyl gallate (PG), tertiary butyl hydroquinone (TBHQ), butylated hydroxyanisole (BHA), and butylated hydroxytoluene (BHT) in food items is described. A C18 column served as the stationary phase; the gradient elution was formed by acetonitrile and water:acetic acid (1%). The UV detector was set at 280 nm. Under the recommended conditions, separation of the four SPAs was achieved in less than 8 min. Analytical characteristics of the HPLC method such as limit of detection, linear range, and reproducibility were evaluated. Extraction parameters were optimized for the recoveries of the SPAs in different types of food items (cooking oil, margarine and butter, and cheese). Before the HPLC separation, the SPAs were extracted with methanol/acetonitrile (1:1, v/v) and were subjected to vortex/ultrasonic treatment. The extracts were next kept in a freezer (∼2 h) to precipitate co-extracted components. Recoveries of the SPAs when spiked to cooking oil, margarine, butter and cheese at 50 and 200 mg l⁻¹ were in the ranges 93.3–108.3% for PG, 85.3–108.3% for TBHQ, 96.7–101.2% for BHA and 73.9–94.6% for BHT. The method was applied to the determination of SPAs in 38 food items (16 cooking oils, ten margarine, six butter and six cheese samples). The levels of SPAs in positive samples are all below the legal limits of Malaysia.     

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.     

Migration analysis,antioxidant, and mechanical characterization of polypropylene-based active food packaging films loaded with BHA,BHT, and TBHQ

Polypropylene (PP) based active composite films were prepared by adding butylated hydroxy anisole (BHA), butylated hydroxytoluene (BHT), and tertiary butylated hydroquinone (TBHQ) antioxidants using the extrusion molding process. All concentrations of BHT, 2% to 3% BHA, and 3% TBHQ significantly increased the tensile strength (TS) of the composite films compared with control films. Increasing antioxidant concentration decreased TS values for BHT films, whereas an opposite trend was observed for BHA and TBHQ films. BHA at < 2%, BHT at > 2%, and TBHQ at all added concentrations significantly reduced elongation at break (E_b) of the composite films compared to control films. Water vapor permeability (WVP) of 1% BHT film was not significantly different from control. However, other antioxidants especially at increased concentrations significantly increased WVP values. TBHQ films with 300% to 662% increase had the highest WVP and BHT films with 5% to 81% increase had the lowest WVP among composite films. All three antioxidants had a negative effect on the transparency of the films; however the effect of BHA at higher concentrations was greater. The antioxidants did not change the color attributes of the films. Films containing all antioxidants showed 2,2-diphenyl-1-picrylhydrazyl radical-scavenging activity, which increased with increase in their concentration, especially for those containing 3 wt.% BHT and TBHQ. Overall, incorporating BHA and BHT into a PP matrix improved mechanical, barrier, antioxidant properties, and film appearance and consequently were proposed for the development of antioxidant active PP films. TBHQ film is not recommended for food packaging because of its weak mechanical properties (lower E_b and TS values, higher WVP, and greater migration).     

Determination and confirmation of five phenolic antioxidants in foods by LC/MS and GC/MS

Identification and determination of butylated hydroxyanisole (BHA), butylated hydroxytoluene (BHT), nordihydroguaiaretic acid (NDGA), propyl gallate (PG) and tert-butylhydroquinone (TBHQ) by means of LC/MS and GC/MS were examined. These five phenolic antioxidants were detected as their pseudo-molecular ions [M-H]- by LC/MS using a Shim-pack FC-ODS column with drying gas. Moreover, BHA, BHT and TBHQ were detected based on their mass fragment ions by GC/MS. Decomposition of TBHQ, NDGA and PG during analysis could be prevented by the addition of L-ascorbic acid (AsA) to the extraction solvent. All five antioxidants were extracted from nikuman, olive oils, peanut butter, pasta sauce and chewing gum with a mixture of acetonitrile-2-propanol-ethanol (2:1:1) containing 0.1% AsA (AsA mixture), which had been cooled in a freezer and filtered. One part filtrate and 5 parts water were mixed and placed on a Mega-Bond Elut C18 cartridge, except in the case of chewing gum. Lipids in foods were removed on a C18 cartridge by washing with 5 mL of 5% acetic acid, and antioxidants were eluted with 5 mL of AsA mixture. The antioxidants spiked into nikuman, olive oil, peanut butter, pasta sauce and chewing gum were successfully identified and their concentrations determined by LC/MS, and GC/MS with good recoveries.     

Effect of BHA, BHT, TBHQ and PG on Growth and Toxigenesis of Selected Aspergilli

The antifungal effect of butylated hydroxyanisole (BHA), butylated hydroxytoluene (BHT), tertiary butylhydroquinone (TBHQ) and propyl gallate (PC) alone or in combination on three toxigenic strains of aspergilli (NRRL 2999, NRRL 4123, NRRL 5835) and three nontoxigenic strains of aspergilli (NRRL 5521, NRRL 5917, NRRL 5918) was examined in a solid medium and in salami. BHT and PG (0.001,0.005,0.01,0.02g per plate) did not inhibit growth, sporulation, and toxigenesis of all six cultures. Aflatoxin production by toxigenic aspergilli (B₁, B₂, G₁ and G₂) in the presence of BHA, TBHQ, and a combination of BHA and TBHQ was reduced significantly (P < 0.05). In salami BHA, TBHQ alone or in combination at 100 ppm significantly (P < 0.05) decreased the aflatoxin production by aspergilli when compared to control samples. A combination of BHA and TBHQ showed synergistic inhibition in both studies (solid medium and salami studies).     

PG、TBHQ、BHA和BHT4种常见抗氧化剂部分稳定性的研究

研究PG、TBHQ、BHA和BHT 4种常见抗氧化剂在不同溶荆、酸碱中稳定性为检测工作者及科研工作者在试验过程中储存或者提取时提供参考依据。采用高效液相色谱法(HPLc),以4种抗氧化剂的保留率为指标,考察4种抗氧化剂的稳定性。从试验结果来看:PG、TBHQ、BHA和BHT在甲醇以及酸性条件下具有较好的稳定性。     

Rapid micropreparation procedure for the gas chromatographic-mass spectrometric determination of BHT, BHA and TBHQ in edible oils

A rapid, accurate and organic solvent saving procedure has been developed for the GC/MS determination of three phenolic antioxidants butylated hydroxytoluene (BHT), butylated hydroxyanisole (BHA) and butyl hydroquinone (TBHQ) in vegetable oils. The method involves two-step microextraction and a centrifugal procedure in a 2 mL autosampler vial, consuming only 50 mg sample and total 1 mL acetonitrile. Recoveries of the phenolic antioxidants when spiked to soya bean oil, peanut oil and cereal cooking oil at 50, 200 and 250 mg/kg, respectively were in the ranges 95.6-104.3% for BHT, 99.7-107.5% for BHA and 93.6-103.8% for TBHQ with the relative standard deviation (RSD) were less than 3% for their independent measurements. The developed method was repeatable and could be applied to determine trace amounts of phenolic antioxidants in vegetable oils.