旋涡振荡萃取- 超高效液相色谱法检测脂肪食品模拟物橄榄油中6 种抗氧化剂

为建立高效且易于操作的脂肪食品模拟物橄榄油中抗氧化剂双酚A(BPA)、叔丁基对羟基茴香醚(BHA)、3,5- 二叔丁基-4- 羟基苯甲醇(Ionox100)、2,6- 二叔丁基对甲酚(BHT)、2,4,6- 三叔丁基苯酚(TTBP)、2,2′- 亚甲基双(4- 乙基-6 叔丁基酚)(AO425)的测定方法,采用旋涡振荡甲醇萃取- 旋转蒸发浓缩以及旋涡振荡乙酸乙酯- 环己烷(1:1,V/V)萃取- 凝胶渗透色谱(GPC)净化浓缩两种前处理方法进行处理,采用超高效液相色谱法(UPLC)检测。结果表明：本方法具有较低的检出限(LODs 分别为0.06、0.04、0.01、0.03、0.06、0.01mg/L)、较好的线性(R2 ＞0.998)、较高的回收率(两种前处理方法平均回收率分别高于83.0%、56.8%)及较高的精密度(RSD 分别小于7.5%、8.4%)。将该方法用于食用油样品的检测,结果显示,只有BHT 被检测出,且含量低于其特定迁移限量(SML)。     

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。     

烟用热熔胶中酚类抗氧化剂的测定

为快速测定烟用热熔胶中的酚类抗氧化剂,以四氢呋喃为良性溶剂提取、甲醇为不良溶剂沉淀基体物质的前处理条件,结合超高效液相色谱(UPLC)建立了烟用热熔胶中苯酚、特丁基对苯二酚(TBHQ)、丁基羟基茴香醚(BHA)、2,4-二特丁基苯酚、2,6-二特丁基苯酚、2,6-二特丁基-4-甲基苯酚(BHT)、四[β-(3,5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯(Irganox 1010)和β-(3,5-二叔丁基-4-羟基苯基)丙酸十八碳醇酯(Irganox 1076)8种酚类抗氧化剂的快速测定方法,并利用该方法测定了10个烟用热熔胶样品。结果表明:(1)方法的回收率为90.9%～103.4%,相对标准偏差(RSD)≤6.7%,检测限为0.008～0.028μg·mL~(-1);(2)烟用热熔胶样品中抗氧化剂以BHT和Irganox 1010为主,未检出苯酚、TBHQ、BHA、Irganox 1076等食品及食品接触材料中常见的抗氧化剂或污染物。该方法简单、快速、准确,适用于烟用热熔胶中酚类抗氧化剂的测定。     

凝胶色谱-气相色谱法测定11种动植物油脂中角鲨烯的含量

动植物食用油经环己烷-乙酸乙酯(1∶1,V/V)萃取后,用凝胶色谱法对油样品进行净化处理,去除样品中大分子的油脂,再采用气相色谱法对动植物食用油中角鲨烯进行测定,以建立多种动植物油中角鲨烯的凝胶色谱-气相色谱(GPC-GC-FID)测定方法。在一定的实验条件下,角鲨烯在9.40~940μg·m L-1范围内呈现良好线性关系,相关系数R2为0.9999,方法回收率为95.7%,RSD为3.0%。该方法处理后的食用油样品中干扰基质少,灵敏度高,可有效避免检测过程中仪器的污染,广泛应用于动植物食用油中角鲨烯的检测,为评判动植物食用油标准提供依据。     

气相色谱-质谱法检测食用油中的邻苯二甲酸酯

建立液-液萃取和固相萃取(SPE)提取方法,结合气相色谱-质谱(GC-MS)联用分析技术,检测食用油中的5种邻苯二甲酸酯类污染物的方法.该方法检测的最低浓度为10ng/g～20ng/g之间,回收率为75%～89%之间,并运用该方法对市售的塑料包装食用油进行了检测.     

油炸小食品中酚类抗氧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小食品中BHA、4HR、BHT、2,2-2甲基双(4-甲基6-叔丁基苯酚) (2246)的含量。采用V(甲醇):V(二氯甲烷)=9:1作提取剂,ODS-2HYPERSIL(250mm×4.6mm,5μm)色谱柱,体积分数80%的甲醇作流动相进行分离。结果表明:浓度在2.0～40μg/mL,4种物质均呈线性关系,相关系数为0.998 3～0.999 1,标准偏差为1.14%～5.90%,平均回收率均在80%以上,检出限2μg/g。因此,该方法可用于油炸食品中酚类抗氧剂的测定。     

高效液相色谱法检测保健食品中的番茄红素

目的建立高效液相色谱法测定保健食品中番茄红素的分析方法。方法用含有0.1%2,6-二叔丁基-4-甲基苯酚抗氧化剂的甲醇:二氯甲烷(10:90,V:V)作为提取溶液。通过Agilent Eclipse XDB-C_(18)(4.6 mm×250mm,5μm)色谱柱;甲醇:乙酸乙酯(85:15,V:V)作为流动相,二极管阵列检测器,检出波长475 nm,色谱柱温25℃,流速1.0 mL/min,进样体积10μL,作为检测条件。结果番茄红素在0~200μg/mL范围内线性良好,相关系数r=0.9995,最低检出限为0.0815μg/mL,平均回收率在89.7%~109.8%之间,RSD为8.4%。结论本方法可以准确、快速地检测保健食品中的番茄红素。     

超声萃取-气相色谱/质谱法测定纺织品中的对叔丁基苯酚北大核心

建立了超声萃取气相色谱/质谱(GC/MS)法测定纺织品中对叔丁基苯酚的方法。样品经超声萃取后,采用气相色谱-质谱仪进行测试分析,以保留时间定性,外标法定量。优化超声萃取条件为:选择甲醇为萃取试剂,萃取时间为30 min,萃取试剂体积为20 mL。对叔丁基苯酚的方法检出限(LOD)为0.05 mg/kg,方法定量限(LOQ)为0.2 mg/kg;在0.1~5.0 mg/L质量浓度范围内方法的线性相关系数R2为0.9998,加标回收率为88.4%~106.3%,相对标准偏差(RSD)为2.37%~7.32%(n=6)。该方法操作简便,准确度高,回收率及精密度好,适用于纺织品中对叔丁基苯酚的测定。     

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。     

乙腈萃取-气相色谱法快速测定食用油中的3种抗氧化剂

本研究旨在建立一种快速、准确的大批量测定食用油中叔丁基羟基茴香醚(Butylated Hydroxyanisole,BHA)、2,6-二叔丁基-4-甲基苯酚(2,6-Di-tert-butyl-4-methylphenol,BHT)和特丁基对苯二酚(Tertiary Butylhydroquinone,TBHQ)含量的气相色谱法。对提取过程中的溶剂、转速和时长进行探究,选择最优提取条件,并用优化后的方法对4种食用油进行3种浓度的加标回收实验。经测定,BHA、BHT和TBHQ的质量浓度在5～100 μg/mL与其色谱峰面积呈较好的线性关系,相关系数R²达到0.999 7以上,方法检出限范围为1.8～4.8 mg/kg,重复性良好。4种食用油的3种浓度的平均加标回收率为85.0%～102.4%,相对标准偏差为1.0%～2.9%(n=6)。该方法快速、简单且试剂消耗少,可用于快速检测大批量食用油样品中的BHA、BHT和TBHQ。该方法还可以为其他样品中的不同抗氧化剂检测提供技术参考。     

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.     

Determination of Four Synthetic Phenolic Antioxidants in Edible Oils by High-Performance Liquid Chromatography with Cloud Point Extraction Using Tergitol TMN-6

A cloud-point extraction (CPE) method using Tergitol TMN-6 (TMN-6) non-ionic surfactant was developed for the extraction and preconcentration of propyl gallate (PG), tertiary butyl hydroquinone (TBHQ), butylated hydroxyanisole (BHA), and butylated hydroxytoluene (BHT) in edible oils. The optimum conditions of CPE were 1.5 % (v/v) Tergitol TMN-6, 1 % (w/v) NaCl, ultrasound-assist 15 min at 49 KHz, 20 min equilibrated at 45 °C, and centrifugation for 10 min at 3,000 rpm. The surfactant-rich phase was then analyzed by reversed-phase high-performance liquid chromatography (HPLC) with ultraviolet detection at 280 nm, under gradient separation, using methanol and 1.5 % (v/v) acetic acid. Under the study conditions, four synthetic phenolic antioxidants (SPAs) were successfully separated within 24 min. Limits of detection in the studied edible oils were in the range of 1.6 to 9.0 ng mL^?1. The high recoveries of the spiked edible oils were obtained in the range 90–98 %. The CPE method has been shown to be a potentially useful methodology for the preconcentration of the target analytes, with a preconcentration factor of 25. This method was compared with cloud point extraction (using Triton X-114) and liquid–liquid extraction (using methanol).     

微波辅助萃取液相色谱快速检测烟草中的多酚类化合物

建立了卷烟烟丝中三个主要多酚化合物(绿原酸、莨菪亭、芸香苷)的超高效液相色谱(UPLC)的快速检测方法.采用微波辅助萃取法(microwave-assisted extraction MAE)分别进行单因素试验和正交试验,确定卷烟烟丝中三个主要多酚类化合物的最佳提取条件:60%(V/V)的甲醇水溶液为提取剂、萃取液温度...     

QuEChERS-超高效液相色谱法测定食用油中5种抗氧化剂

为快速准确测定食用油中抗氧化剂含量,通过QuEChERS-超高效液相色谱法建立同时测定食用油中丁基羟基茴香醚(BHA)、特丁基对苯二酚(TBHQ)、二丁基羟基甲苯(BHT)、没食子酸丙酯(PG)、没食子酸辛酯(OG)5种常见抗氧化剂含量的方法。样品先采用甲醇溶解提取,提取液经冷冻离心、净化剂净化分离后上机检测,超高效液相色谱仪以乙腈-水为流动相进行梯度洗脱,采用外标法定量。结果表明：5种抗氧化剂在1.0～100.0 mg/L范围内线性关系良好,检出限均不大于1.6 mg/kg,加标回收率在85.78%～100.85%之间,RSD在2.40%～6.01%之间。综上,该方法具有操作简单、重现性好、灵敏度高等特点,适合动植物油中5种常用抗氧化剂含量的检测与分析。     

固相萃取- 高效液相色谱检测法测定食用菌中三聚氰胺残留量

建立食用菌中三聚氰胺的固相萃取- 高效液相色谱检测法。样品经三氯乙酸、乙腈提取,离心,混合型固相萃取小柱净化后,过0.45μm 滤膜,用配有二极管阵列检测器(PAD)的液相色谱仪检测,外标法定量。同时,以三聚氰胺标准品进行添加回收率测定,结果显示,本方法对三聚氰胺的测定低限为2.0mg/kg,回收率为81.3%～91.7%,测定的相对标准偏差均不大于5.6%。本方法能满足食用菌中三聚氰胺残留量常规检测的需要。     

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.     

食用油脂中合成抗氧化剂的检测分析研究进展

向油脂中添加合成抗氧化剂是防止食用油脂在使用过程中发生氧化酸败的最有效方法之一,国家规定油脂中合成抗氧化剂添加的最大限量标准为200 mg/kg,因此建立准确、快速和高效的分析方法检测食用油脂中合成抗氧化剂的含量保证油脂以及含油食品的质量安全具有十分重要的意义。食用油脂中抗氧化剂的检测方法较多,最常用的有高效液相色谱法、气相色谱法、高效液相色谱-串联质谱法、气相色谱-串联质谱法等。本文主要综述了近年来食用油脂中合成抗氧化剂检测分析方法的研究进展,总结了不同分析方法之间的差异,并对今后的发展趋势加以展望。     

Solid-Phase Extraction and Procedure for Determination of Phenolic Compounds in Maple Syrup

A solid phase extraction procedure was developed for the extraction of phenolic compounds from maple syrup. The list of targeted chemicals contains phenolic acids as well as aldehydes, flavanols and others such as coniferyl alcohol and 5-hydroxymethyl furfural. The procedure consists in passing a small quantity of maple syrup, 1 g diluted in 2 ml deionized water, through an Oasis HLB cartridge of 200 mg. The cleanest extracts were obtained by rinsing the cartridge load with formic acid 2 %/methanol (9:1). The analytes eluted with methanol were passed in an high-performance liquid chromatography (HPLC)-DAD system for analysis. The method performances show good recoveries; excluding gallic acid measured at 49 %, the chemical recoveries ranged from 81 to 119 %. Moreover, the method repeatability is less than 12 % (RSD) relative standard deviation for all chemicals except for epicatechin (20 %). The analysis method was applied for the determination of phenolic compounds in maple syrups from different color classes (Extra Light to Amber). Results show that concentrations of phenolic compounds vary among syrup classes and the greatest concentration was observed for the Amber syrups.     

菜籽油低共熔溶剂萃取物抗氧化活性研究

以菜籽油为材料,DPPH自由基清除活性为指标,比较了氯化胆碱-尿素、氯化胆碱-甘油、氯化胆碱-乙酰丙酸3种低共熔溶剂(DES)和80%甲醇萃取物的抗氧化活性,筛选出最优的低共熔萃取剂,并分析了其与80%甲醇萃取物的抗氧化成分差异。研究表明：氯化胆碱-乙酰丙酸低共熔溶剂菜籽油萃取物的抗氧化活性显著高于80%甲醇萃取物,而氯化胆碱-尿素和氯化胆碱-甘油低共熔溶剂萃取物的抗氧化活性低于80%甲醇。通过总酚含量测定、薄层层析-DPPH显色、HPLC等方法,比较了氯化胆碱-乙酰丙酸低共熔溶剂和80%甲醇萃取物成分的差别,氯化胆碱-乙酰丙酸低共熔溶剂萃取物的总酚含量是80%甲醇的143.27%,抗氧化物质的种类和数量也比80%甲醇萃取物有显著的提升。因此氯化胆碱-乙酰丙酸低共熔溶剂可用于植物油脂抗氧化成分萃取和分析。