Determination of Bisphenol A diglycidyl ether (BADGE) and its hydrolysis products in canned oily foods from the Austrian market

 Bisphenol A diglycidyl ether (BADGE) is determined in canned oily foods from Austria using a new simplified HPLC method. Samples are extracted with pentane, back extracted with methanol, and finally dissolved in the mobile phase (cyclohexane/tert–butyl methyl ether). Separation is performed on a normal-phase HPLC column using fluorescence detection. Verification of the BADGE-containing peak is carried out by using off-line GC-MS. Additionally, the synthesis and determination of BADGE hydrolysis products, Bisphenol A bis(2,3-dihydroxypropyl) ether (BADGE.2H₂O) and Bisphenol A glycidyl (2,3-dihydroxypropyl) ether (BADGE.H₂O) are presented. From 67 analyzed cans, containing various fatty meat or fish products, 16% were above the maximum quantity of 1 mg/kg tolerated by the European Community, 45% were in the range between 0.1–1 mg/kg, 24% between 0.02 and 0.1 mg/kg, and in 15% the BADGE concentrations were below the detection limit of 0.02 mg/kg. The hydrolysis product BADGE.H₂O was not detected in any sample, whereas BADGE.2H₂O was found in some samples up to a concentration of 0.5 mg/kg. Received: 11 May 1998 / Revised version: 1 July 1998     

高效液相色谱法同时测定食品中9种水溶性维生素

目的建立同时测定食品中9种水溶性维生素的高效液相色谱分析方法。方法采用C18色谱柱进行分离,以pH 2.5,25 mmol/L KH2PO4-乙腈二元体系为流动相进行梯度洗脱,最后用高效液相色谱二极管阵列检测器对9种维生素进行测定。结果在优化实验条件下,测得维生素C的线性范围为0.04~100μg/mL,硫胺、核黄素、烟酰胺和吡哆醇的线性范围为0.02~100μg/mL,泛酸的线性范围为0.08~400μg/mL,生物素的线性范围为0.08~200μg/mL,叶酸的线性范围为0.01~50μg/mL,氰钴胺的线性范围为0.04~100μg/mL;线性相关系数为0.9997~0.9999,相对标准偏差为0.28%~1.35%,检出限范围为3~45 ng/mL,加标回收率为90.6%~105.4%。结论该方法快速、准确、灵敏,适合测定营养强化食品中多种水溶性维生素。     

基于HPLC法对罐装食品中双酚A的测定方法研究

采用中空纤维—液相微萃取—高效液相色谱法(HF—LPME—HPLC)对罐装食品中的双酚A含量进行测定,优化萃取剂、样品溶液pH值、萃取温度、萃取时间以及搅拌速率等基本数据参数,旨在建立一种简便、快捷、准确的检测方法。研究结果表明:以正辛醇为萃取剂,其选取的测定食品样本溶液pH值为6.1,而相应的萃取温度则为40℃,时间为40min,相对标准偏差为4.3%,检测限为12.7μg/L,食品样本中双酚A的富集倍数达到了200倍,样品平均回收率达到了86.1%~105%。     

反相HPLC法同时测定烟草中的6种有机酸

建立了用反相高效液相色谱法同时快速测定烟草中柠檬酸、苹果酸和草酸等6种有机酸的方法。采用的色谱柱为Hypersil C18(250mm×4.6mm,5μm),流动相0.01mol/L NaH2PO4(pH2.98)和无水甲醇(体积比为98∶2),流速为1.0mL/min,柱温25℃,检测波长210nm。有机酸的回收率为98.2%~104.3%;相对标准偏差为0.61%~3.38%;检出限0.04~0.53μg/mL,分析时间不超过7min。并分析了4种转光地膜和普通地膜覆盖的K326初烤烟叶中这6种有机酸的含量。     

高效液相色谱法同时测定食品中10种合成着色剂

目的 建立一种高效液相色谱法同时测定食品中10种合成着色剂(柠檬黄、新红、觅菜红、靛蓝、胭脂红、日落黄、诱惑红、亮蓝、喹琳黄、赤藓红).方法 用GB/T 5009.35-2003(食品中人工合成着色剂的测定方法)中试样处理方法制备样品溶液,聚酰胺吸附法提取色素,以甲酵/乙睛(3+1)+乙酸铵(0.02 mol/L,pH =4.0)为流动相,梯度淋洗分离,多波长检测定量.结果 线性范围分别为柠檬黄、觅菜红、靛蓝、胭脂红、日落黄于0.94-30.00p.g/ml,新红于0.94～30.00μg/ml,诱惑红于1.00～32.10μg/ml,亮蓝于0.31～10.00μg/ml,喹琳黄于1.219.68μg/ml,赤藓红于0.76～24.40μg/ml,线性关系良好,相关系数0.999 0～1.000 0,回收率87.5% - 101.4%,RSD 1.3%～5.7%,检出限分别为0.03～ 0.9 mg/kg.结论 该方法简单、准确、灵敏,适用于食品中10种合成着色剂的定量分析.     

食品中蔗糖检测方法的研究

采用高效液相色谱仪(配示差折光检测器),摸索出对食品中蔗糖测定的色谱条件和前处理方法,进行准确定量测定的研究。标准曲线有较好的线性关系,方法回收率在95%～105%之间;RSD<3.0%,精密度高;方法最低检出限为0.9g/kg,方法定量限为3.0g/kg。     

HPLC法测定食品中的叶黄素含量

为了测定食品中的叶黄素的含量,建立方便可靠的测定方法,采用高效液相色谱法对食品中叶黄素含量进行了测定.使用硅胶色谱柱(4.6mm×250 mm,5μm),以环己烷∶乙酸乙酯=75 ∶ 25为流动相,检测波长445nm.该方法最低检出量1.0mg/kg,RSD 为1.2%,加标回收率为93.85.6%,RSD 为3.1%～4.1%.该方法简便、准确,有良好的重现性,技术参数指标符合食品理化分析的要求.     

HPLC法测定食品中的叶黄素含量

为了建立测定食品中的叶黄素含量的可靠方法,采用高效液相色谱法进行了测定.使用硅胶色谱柱(4.6 mm×250 mm,5μm),以环己烷∶乙酸乙酯=75∶25为流动相,检测波长445nm.该方法最低检出量1.0 mg/kg,RSD为1.2%,加标回收率为93.8%～105.6%,RSD为3.1%～4.1%.该方法简便、准确,有良好的重现性,技术参数指标符合食品理化分析的要求.     

高效液相色谱法同时测定食品中9种合成着色剂

目的建立高效液相色谱法(high performance liquid chromatography, HPLC)同时检测食品中9种合成着色剂(柠檬黄、新红、苋菜红、靛蓝、胭脂红、日落黄、诱惑红、亮蓝及酸性红)的分析方法。方法样品经超声提取、聚酰胺净化、浓缩、定容、过膜,经Shim-pack GIST C18色谱柱(250 mm×4.6 mm, 5μm)分离,以甲醇和0.02mol/L乙酸铵为流动相,梯度洗脱分离进二极管阵列检测器检测。结果在0.4～20.0μg/mL浓度范围内,线性关系良好,相关系数均在0.999以上,方法检出限为0.5mg/kg;分别对多种样品进行低(0.5 mg/kg)、中(1.0 mg/kg)、高(5.0 mg/kg) 3个浓度加标回收率实验,回收率范围为76.2%～107.1%,相对标准偏差(relative standard deviations, RSDs)为0.4%～8.5%(n=6)。结论该方法分析速度快、准确度高、重复性好,适用于各种基质食品中9种合成着色剂的同时检测。     

罐头涂料铁罐双酚A二缩水甘油醚及其衍生物迁移规律研究

研究了罐头涂料铁罐双酚A二缩水甘油醚及其衍生物在特定食品模拟物中的迁移规律。采用50%（v/v）乙醇溶液为食品模拟物,应用高效液相色谱-串联质谱法进行双酚A二缩水甘油醚及其衍生物的定性定量分析,并应用基于Fick扩散第二定律的D.Chung模型和基于概率与数理统计方法的Weibull模型进行了预测。结果表明:贮存条件对迁移总量变化影响显著,温度越高越快达到平衡,迁移平衡值为1.28 mg/kg;D.Chung模型中扩散系数D与贮存温度符合阿伦尼乌斯动力学模型,该模型预测值与实验值的拟合优度（R²）小于0.23,而Weibull模型拟合优度（R²）能达到0.90以上。因此,Weibull模型比D.Chung模型更接近实际迁移结果,为评估涂料铁罐的安全性提供参考。      

Chlorohydrins of bisphenol A diglycidyl ether (BADGE) and of bisphenol F diglycidyl ether (BFDGE) in canned foods and ready-to-drink coffees from the Japanese market

BADGE.2HCl and BFDGE.2HCl were determined in 28 samples of ready-to-drink canned coffee and 18 samples of canned vegetables (10 corn, 5 tomatoes and 3 others), all from the Japanese market. HPLC was used as the principal analytical method and GCMS for confirmation of relevant LC fractions. BADGE.2HCl was found to be present in one canned coffee and five samples of corn, BFDGE.2HCl in four samples of canned tomatoes and in one canned corn. No sample was found which exceeded the 1mg/kg limit of the EU for the BADGE chlorohydrins. However the highest concentration was found for the sum of BFDGE.2HCl and BFDGE.HCl.H₂O at a level of 1.5mg/kg. A Beilstein test confirmed that all cans containing foods contaminated with BADGE.2HCl or BFDGE.2HCl had at lest one part coated with a PVC organosol.     

食品中果聚糖的测定方法研究进展

果聚糖天然存在于菊苣、菊芋、香蕉、大蒜、洋葱、大麦等多种植物中,作为一种水溶性膳食纤维广泛应用于婴幼儿食品、乳制品、饮料、焙烤食品等,且果聚糖具有与普通食糖迥然不同的消化过程和代谢途径,并具有多种生理功能,一直是国内外生产企业和科研院所关注的热点。由于果聚糖的聚合度不同,且存在不同的化学结构形式,一些明确化学结构式的成分缺少对照品,因此定性定量分析有很大的难度。近年来,国内外科研人员在分析检测方面做出了不懈的努力,建立了多种检测方法。本文对果聚糖的分类、结构和应用进行了概述,并总结了各种检测方法的优缺点,为生产企业、检验检测机构人员选择检测方法提供技术支持,为精准定量食品中的果聚糖含量提供参考。     

高效液相色谱法同时测定果蔬汁中脱氢乙酸与纳他霉素及其降解规律研究

目的建立高效液相色谱法(high performance liquid chromatography,HPLC)同时测定果蔬汁中的脱氢乙酸与纳他霉素。方法样品采用超声提取,以乙腈与0.1%甲酸-水溶液为流动相进行梯度洗脱,经过C_(18)色谱柱分离,采用二极管阵列检测器检测,检测波长为310 nm和305 nm,以外标法定量。结果脱氢乙酸与纳他霉素在0.01~20μg/m L浓度范围内线性关系良好(r~2=0.99987),定量限分别为1.0 mg/kg和0.5 mg/kg,均小于等于国标方法定量限。脱氢乙酸与纳他霉素分别在5、10和50 mg/kg及0.5、1和5 mg/kg 3个水平加标回收率分别为92.44%~95.02%和91.20%~103.49%,实验室内部变异系数分别为0.28%~0.43%和0.78%~10.44%。与国标方法对比,在置信度为95%时的显著性检验结果较好。研究脱氢乙酸和纳他霉素的降解规律发现,脱氢乙酸自身降解较慢,且受到样品基质影响较小;而纳他霉素自身降解较快,且受到样品基质影响较大。结论本方法准确可靠,精密度良好,可用于果蔬汁样品中脱氢乙酸与纳他霉素的同时测定。     

Migration of bisphenol-A diglycidyl ether (BADGE) and its reaction products in canned foods

Bisphenol-A diglycidyl ether (BADGE) is used as an additive or starting agent in coatings for cans. The presence of hydrochloric acid in the organosol (PVC-based) lacquers results in formation of chlorohydroxy compounds of BADGE. These compounds, as well as BADGE itself, are potential migrants into the preserved food and are of toxicological concern. In the present investigation the presence of BADGE and the chlorohydroxy compounds (BADGE.HCl and BADGE.2HCl) in various kinds of canned foods from 30 brands have been determined by HPLC with fluorescence detection. BADGE was found in levels up to 5.1mg/kg in the food and only in food from cans containing BADGE.HCl and BADGE.2HCl in the lacquers. BADGE was found both in fish in oil and in fish in tomato sauce, however, the highest amounts were found in the fatty foodstuffs. BADGE.HCl and BADGE.2HCl were found in concentrations up to 2.4mg/kg and 8.3mg/kg, respectively. Unlike BADGE, BADGE.2HCl was found in similar concentrations in fish in oil and in fish in tomato sauce. In aqueous and acidic foodstuffs BADGE readily hydrolyses into mono- and dihydrolysed products (BADGE.H₂O and BADGE.2H₂O). In this study BADGE.H₂O was not found in any food sample, whereas BADGE.2H₂O was found in levels up to 2.6mg/kg. The Scientific Committee for Food (SCF) of the European Commission has proposed that a limit of restriction of 1mg/kg food shall include BADGE itself and BADGE.H₂O, BADGE.HCl, BADGE.2HCl and BADGE.HCL.H₂O. The present results indicate that the migration of BADGE.HCl and BADGE.2HCl, compounds with almost no data on toxicity, implies a greater problem than BADGE.H₂O and BADGE.2H₂O.     

Determination of bisphenol A in canned fatty foods by coacervative microextraction,liquid chromatography and fluorimetry

Decanoic acid reverse micelle-based coacervates were used to provide simple, rapid and almost solventless extraction of bisphenol A (BPA) from canned fatty foods. The procedure involved the extraction of 200–400 mg of homogenised food sample with an aqueous solution containing 20% THF and 200 mg of decanoic acid, conditions under which the coacervate (around 550 µl) formed in situ and instantaneously. The overall sample treatment took about 30 min and several samples could be simultaneously treated using conventional laboratory equipment. No clean-up or solvent evaporation were required before determination of BPA by liquid chromatography and fluorescence detection. Recoveries in samples were between 90 and 99%, with relative standard deviations in the range 2–7%. The limit of quantification ranged 29–15 ng g^?1 for 200–400 mg of sample, being far below the current specific migration limit (SML) set by the European Commission (600 ng g^?1). The method was successfully applied to the determination of BPA in the solid content of canned fish (from 20 to 129 ng g^?1) and meat (from undetected to 37 ng g^?1).     

超高效液相色谱同时测定食品中4种工业染料

目的建立同时测定食品中酸性橙、碱性橙、碱性嫩黄、罗丹明B工业染料的方法。方法样品用水-5%氨水乙腈-正己烷混合溶剂提取净化,采用ZORBAX Extend C18(2.1 mm i.d.×50 mm,1.8μm)分离,以乙腈—乙酸铵缓冲液梯度洗脱,流速为0.5 ml/min,二极管阵列检测器检测酸性橙(λ=485 nm)、碱性橙及碱性嫩黄(λ=435nm)、罗丹明B(λ=548 nm)。结果 4种组分在0.1～10.0 mg/L范围内有良好的线性关系(r>0.999),检测限为0.006 4～0.019 mg/kg。在番茄沙司、腊肠、辣椒油3种不同食品基质中平均加标回收率为70.0%～102.7%,相对标准偏差为0.5%～3.1%。结论方法快速,简单,可应用于食品中酸性橙、碱性橙、碱性嫩黄、罗丹明B 4种工业染料的同时检测。     

重氮化偶合HPLC法测定食品中的亚硝酸盐含量

探讨了食品中亚硝酸盐含量的重氮化偶合高效液相色谱测定方法.食品样品除去蛋白质、脂肪后,亚硝酸盐与对氨基苯磺酸重氮化,再与N-1-萘基乙二胺偶合,之后进行HPLC分析.以SB-C18柱为分离柱,VWD和DAD为检测器,乙酸溶液(14%)/甲醇(80:20)为流动相,流速为1.0mL/min,检测波长为544nm,进样20μL.在10～1000ng/mL范围内,亚硝酸盐含量与峰面积呈良好线性关系(r=0.9997).方法最低检测浓度为40μg/kg.     

高效液相色谱法测定水果罐头中阿斯巴甜的不确定度评估

目的评定高效液相色谱法测定水果罐头中阿斯巴甜含量的不确定度。方法按照GB 5009.263-2016《食品安全国家标准食品中阿斯巴甜和阿力甜的测定》测定水果罐头中阿斯巴甜,根据JJF 1059.1-2012《测量不确定度评定与表示》的方法,建立高效液相色谱法测定水果罐头中阿斯巴甜不确定度评定的数学模型,分析其中各不确定度分量的来源,并对其分别进行量化,最终合成水果罐头中阿斯巴甜含量测定结果的不确定度。结果水果罐头中阿斯巴甜含量测定结果 0.0926 g/kg时,在95%的置信区间下,扩展不确定度为0.00282g/kg(k=2)。结论实验过程的不确定度主要来源引有标准溶液的配制操作、标准曲线的拟合过程、试样定容、重复性测定等。     

高效液相色谱法快速检测食品中18种合成色素

建立了一种HPLC法同时检测食品中柠檬黄、苋菜红、靛蓝、胭脂红、日落黄、罗丹明B、喹啉黄、皂黄、碱性橙Ⅱ、碱性嫩黄O、诱惑红、偶氮玉红、赤藓红、酸性橙Ⅱ、碱性橙21、碱性橙22、亮蓝、专利蓝等18种水溶性合成色素的分析方法。采用直接溶剂提取法,以Venusil MP C18柱（4.6mm×250mm,5μm）为分析柱,甲醇-乙腈（1∶1）-0.02mol/L乙酸铵溶液为流动相,采用梯度洗脱进行分离,以二级管阵列检测器检测（扫描范围:200⁸00nm）,外标法定量。结果显示,18种色素在0.5²0.0mg/L范围内具有良好的线性,相关系数（r）均大于0.9980,在3、15、40mg/kg三个加标水平下的平均回收率为68.9%¹00.8%,相对标准偏差（n=6）为0.1%⁵.3%,检出限为0.06³.75mg/kg。将建立的方法应用于市场上部分有色食品的筛查,结果证明该方法前处理步骤简便,色谱分离效果好,适合多种食品中合成色素的检测;对部分食品样品进行检测发现,有色食品中使用合成色素较为普遍。      

高效液相色谱法同时测定紫丁香苷、绿原酸、栀子苷和红景天苷的含量

目的建立高效液相色谱法同时测定紫丁香苷、绿原酸、栀子苷和红景天苷的含量。方法样品经过前处理,以0.05%磷酸水:乙腈:甲醇(85:10:5,V:V:V)为流动相,等度洗脱,经反相硅胶柱(4.6 mm×150 cm,5μm)分离,并于220 nm波长检测。结果紫丁香苷在浓度1.0~51μg/m L之间呈现良好的线性关系,r=0.9995,平均回收率为99.16%~99.32%,相对标准偏差为0.10%;绿原酸在浓度5.3~27μg/m L之间呈现良好的线性关系,r=1.0000,平均回收率在99.08%~99.51%之间,相对标准偏差为0.23%;栀子苷在浓度6.1~30μg/m L之间呈现良好的线性关系,r=0.9990,平均回收率在98.16%~98.38%之间,相对标准偏差为0.13%;红景天苷在浓度5.3~26μg/m L之间呈现良好的线性关系,r=0.9990,平均回收率在98.75%~99.86%之间,相对标准偏差为0.58%。结论该方法能同时测定紫丁香苷、绿原酸、栀子苷和红景天苷含量,耗时短、操作简便、准确、重现性好,可在实验室推广。