液相色谱-串联质谱法检测食品中合成染料的研究进展

合成染料由于价格低廉、着色能力强和性质稳定等特点而被广泛用于赋予和改善食品色泽, 但合成染料的滥用问题如超范围使用、超限量使用以及违法使用会对消费者的健康造成不利影响, 因此需要高灵敏度和高准确度的分析方法来检测食品中的合成染料, 以确保食品安全。液相色谱-串联质谱法具有高选择性、高灵敏度和准确性等优点, 在合成染料定性和定量分析中发挥着重要作用。本文综述了液相色谱-串联质谱法在食品中合成染料检测的研究进展, 涉及合成染料的样品前处理方法、色谱分离方法和质谱检测方法, 并对液相色谱-串联质谱技术在合成染料检测领域未来的发展趋势进行了展望, 为今后合成染料检测的方法开发提供参考和思路。     

Food colors: Existing and emerging food safety concerns

Food colors are added to different types of commodities to increase their visual attractiveness or to compensate for natural color variations. The use of these additives is strictly regulated in the European Union, the United States, and many other countries worldwide. There is a growing concern about the safety of some commonly used legal food colorants and there is a trend to replace the synthetic forms with natural products. Additionally, a number of dyes with known or suspected genotoxic or carcinogenic properties have been shown to be added illegally to foods. Robust monitoring programs based on reliable detection methods are required to assure the food is free from harmful colors. The aim of this review is to present an up to date status of the various concerns arising from use of color additives in food. The most important food safety concerns in the field of food colors are lack of uniform regulation concerning legal food colors worldwide, possible link of artificial colors to hyperactive behavior, replacement of synthetic colors with natural ones, and the presence of harmful illegal dyes—both known but also new, emerging ones in food. The legal status of food color additives in the EU, United States, and worldwide is summarized. The reported negative health effects of both legal and illegal colors are presented. The European Rapid Alert System for Food and Feed notifications and US import alerts concerning food colors are analyzed and trends in fraudulent use of color additives identified. The detection methods for synthetic colors are also reviewed.     

软饮料中人工合成色素快速测定试纸条的研制

基于聚酰胺薄膜与人工合成色素之间的特异性吸附的原理,建立一种快速、低成本的测定软饮料中最常用的3种人工合成色素(胭脂红E124、柠檬黄E102、日落黄E110）的方法。在优化后的检测条件下,3种色素的最低检测限分别为0.4、0.3mg/L和0.4mg/L,检测时间10min。对14个市售样品进行检测,结果表明,建立的快速检测方法与薄层色谱和高效液相色谱两种方法的结果吻合。该方法操作简单、不需要仪器设备,凭肉眼判读,可用于现场检测和快速筛查,为控制和监测合成色素的滥用或过量添加提供技术途径。     

阴离子染料吸附剂ADA—4用于污水脱色的研究

本文对阴离子染料吸附剂ＡＤＡ－４吸附、解吸和再生性能及机理进行了研究。实验结果表明，ＡＤＡ－４吸附剂用于印染污水脱色，不但对污水中的阴离子染料有很强的吸附能力，大大降低了污水色度，而且还可以通过既简单双经济的方法使吸附剂－载体上的解吸，使其吸附性能再生。     

Determination of three dyes in commercial soft drinks using HLA/GO and liquid chromatography

Allura Red, Sunset Yellow, and Tartrazine usually present in commercial soft drinks were accurately quantified using HLA/GO method, a net analyte signal-based method, without the need for solutes separation. The obtained percent recoveries (R.S.D.) of dyes were 99.8 (2.8), 102 (3.3), and 100 (4.5) for Allura Red, Sunset Yellow, and Tartrazine, respectively. The calibration method was applied for analysis of food dyes in powdered soft drinks with minimum sample preparation measures. The proposed HLA/GO method was validated against a standard HPLC method. Statistical analyses showed insignificant differences between the results of two methods. The developed HLA/GO method offers a simple and rapid procedure for determination of food dyes in powdered soft drinks in comparison with HPLC methodology.     

Determination of synthetic dyes in selected foodstuffs by high performance liquid chromatography with UV-DAD detection

A relatively fast method was developed and applied to the determination of selected synthetic food dyes (Sunset Yellow, Tartrazine, Amaranth, Brilliant Blue and Red-40) in three different kinds of foodstuffs: solid juice powders, solid jelly powders and soft drinks. High performance liquid chromatography with UV-DAD detection was employed. The developed chromatographic method employed an ODS Zorbax column (250 mm; 4.6 mm; 5 μm). Two different solvent systems were employed depending on the expected dyes in the studied samples. Sample preparation consisted of dissolving and filtering the samples and showed high throughput. Adequate detection and quantification limits together with high recoveries (better than 98.8%) were obtained. All studied samples showed dye levels in conformity with Brazilian legislation. Indeed some products showed poor quality and/or production controls due to the variability between lots. This fact was more critical for Tartrazine and Sunset Yellow in solid juice powders and there is concern that these substances can exceed legislated values. It was also observed that different producers use different dyes and/or composition in similar products.     

Determination of synthetic food dyes in food by capillary electrophoresis

A method for the determination of 12 synthetic food dyes (Amaranth, Erythrosine, Allura Red AC, New Coccine, Phloxine, Rose Bengal, Acid Red, Tartrazine, Sunset Yellow FCF, Fast Green FCF, Brilliant Blue FCF, Indigo Carmine) in food was developed using capillary electrophoresis (CE) with photodiode array detection. The dyes were extracted with water and 0.5% ammonia-ethanol (1:1) mixture, and cleaned up using solid-phase extraction (Sep-Pak Plus tC18). The dyes were eluted with methanol from the cartridge. The dyes were separated by CE on a bubble cell fused-silica capillary (72 cm to the detector, 75 microm i.d.) using 20% acetonitrile in a mixture of 10 mmol/L potassium phosphate, monobasic and 5 mmol/L sodium carbonate (pH 10.0) as the running buffer. Identifications of the dyes were performed on the basis of the migration time and the absorbance spectrum of each peak. The coefficients of variation of the migration times and the peak areas were 0.28-0.62% and 1.84-4.30%, respectively (n = 5). The identification limits using the absorbance spectra of the dyes were 10 microg/mL for Brilliant Blue FCF and Fast Green FCF, and 5 microg/mL for the other 10 dyes. The recoveries of the 12 dyes from pickles, soft drinks and candies at the level of 10 microg/g were 70.0-101.5%. The method was applied to the analysis of dyes in foods. The dyes detected by CE were in agreement with those detected by paper chromatography.     

Liquid chromatographic quantification of synthetic colorants in fish roe and caviar

According to the directive 94/36/EC of the European Union (EU), quantities of synthetic colorants added to foods are restricted by upper limits and, therefore, reliable methods for their quantification have to be established. Approved colorants, defined by so-called E numbers, are permitted for dying fish roe (commonly named caviar). We developed a chromatographic method for the quantitation of colorants in roe. The recovery rates of 14 synthetic food colorants from solid materials (Al₂O₃, XAD-2, anion exchangers, and polyamide-6) were tested, and polyamide powder was selected as adsorbent for quantitative determination of colorants in fish roe. The most effective sample preparation comprises extraction of colorants from roe with 1 M aqueous ammonia, defatting of the solution with n-hexane, adjustment of pH 2 of the extract, adsorption of dyes on the polyamide and desorption with a mixture of aqueous ammonia (25%) and methanol (1:9 v/v). The isolated colorants were analyzed by RP-HPLC with diode-array detection. In several caviars, the maximum of individual colorants regulated by EU were exceeded or colorants declared on food labels were not detected. Presented at 25th International Symposium on Chromatography, Paris, France, October 4–8, 2004.     

果汁饮料中合成色素检测方法的改进

目的:本实验通过对国标中合成色素检测前处理方法的改进,考察了吸附解吸装置、洗脱剂中氨水比例、聚酰胺粉用量、旋转蒸发温度对实验结果的影响,建立了测定果汁饮料中柠檬黄、日落黄的HPLC检测方法.方法:样品经聚酰胺粉吸附,甲醇—甲酸溶液除去天然色素,乙醇—氨水—水混合溶液(5:4:1)洗脱,70℃旋干溶液,复溶后经C18液相色谱柱分离,甲醇-0.02mol/L乙酸铵溶液(pH=4)梯度洗脱,紫外检测器检测.结果:柠檬黄的检出限为0.2mg/kg,日落黄的检出限为0.3mg/kg.柠檬黄和日落黄的回收率均＞99.0％.结论:该方法稳定性好、回收率高、适用范围广,可用作复杂基质中多种合成色素的同时检测.     

Synthetic colourings of some snack foods consumed by primary school children aged 8–9 years in Hong Kong

An HPLC method with photodiode array detection was used for the quantification of 11 synthetic dyes in 87 snack food products commonly consumed by children in Hong Kong, China. Dietary exposure to synthetic colours was estimated using food-frequency questionnaire data obtained from 142 primary school children aged 8–9 years in three districts of Hong Kong. Dietary exposure to synthetic colours for an average primary school student was considerably lower than the threshold for acceptable daily intake (ADI) for their ages, except for sunset yellow FCF. Data obtained showed that the average daily intake of sunset yellow FCF (E110) was 51% over the ADI threshold in 9-year-old boys. The higher intakes of sunset yellow FCF were mainly due to the high consumption of soft drinks and desserts such as jellies, which have high concentrations of this synthetic colour additive.     

用于食品质量监测的pH智能指示剂的研究进展

近年来,消费者对于食品安全要求的改变促进了包装新技术的发展。目前用于食品质量监测的智能包装技术主要有指示剂、数据载体装置以及传感器等。其中,pH智能指示剂由于其成本低、体积小、制备方便和指示效果好等优点而成为研究热点。通常来说,指示剂是由负载基和pH染料组成。同时天然pH染料如茜素、姜黄素、类胡罗卜素、花青素等对于环境酸碱性的改变能表现出明显的颜色变化。以天然pH染料制备的pH智能指示剂能够传递食品的实时信号（颜色、化学或电子）,以表现实时的质量信息。本文主要对以天然染料和生物聚合物为基础的pH智能指示剂的研究现状进行了概述,讨论了基于天然pH染料和合成pH染料相比的pH智能指示剂的重要性,以及未来的研究趋势。     

顶空气相色谱法测深色酒中微量甲醇

甲醇是酒精饮料中的有害成分 ,其检测方法主要有品红亚硫酸比色法和气相色谱法两种 ,但由于像有色酒和药酒等颜色较深、成分复杂的酒 ,品红亚硫酸比色法的误差及重现性均较差 ,而采用气相色谱法直接进样又极易污染顶色谱柱。因此 ,在检测前对样品必须进行蒸馏或多次蒸馏或其它预处理。采用HSGC法测定了五种深色酒中微量甲醇 ,避免了样品的预处理且方法简便、快速且准确性和重现性均较好     

食品中偶氮类色素检测方法的研究进展

食品在加工的过程中容易丢失原本的颜色,食品加工者为了使食物看起来更美味,向其中添加廉价的合成色素。但偶氮类合成色素对人体存在致癌风险,许多国家已禁止在食品中添加偶氮类合成色素,并严格监管该类食品在国内的流通及进出口。本文综述了食品行业中针对偶氮类合成色素的各种检验方法,以期为食品安全监督检测相关机构提供参考。当前国内外食品中禁用偶氮色素检验方法主要包括光谱法、色谱法、电化学、酶联免疫法、化学发光及其他检测方法等,这些方法在方便、快捷、准确等方面取得了较大的进步,但是仍然面临一些问题,如灵敏度低、定性能力差、假阳性率高,成本高和前处理复杂等。因此开发操作简便、高通量的检测技术和仪器将是未来的发展方向。     

高职女生饮食习惯与肥胖问题的调查与分析

目的:了解并分析北京某高职院校女生的饮食习惯和肥胖问题,为科学指导合理膳食和调控体重提供科学依据。方法:随机选取150名高职女生,进行膳食调查与人体测量,对高职女生的体质指数、减肥行为、饮食习惯等进行调查,所得数据进行统计分析。结果:高职女生肥胖的检出率较高,对自我体重评价的正确率低,普遍具有减肥的意愿,减肥方法不科学;绝大多数高职女生有吃夜宵的习惯,而且夜宵食物的选择不科学;经常吃洋快餐、油炸食物,经常喝酒、喝饮料,进食速度快的高职女生所占比例较高。结论:高职女生肥胖检出率较高,需要进行体重调控;高职女生存在不良的减肥行为和饮食习惯,应有针对性地开展积极有效的营养健康教育,以纠正和建立良好的饮食习惯,科学调控体重。     

饮料中柠檬黄的测定能力验证情况分析

目的了解和评价全国食品检验系统实验室对人工合成着色剂柠檬黄的检测能力,促进各参加实验室在人工合成着色剂检测方面能力的提高。方法在全国食检系统内组织开展饮料中柠檬黄的测定能力验证项目。制备阳性及空白考核样品,完成均匀性稳定性实验,确保样品满足能力验证发样要求,向167家参加实验室随机发放样品,并在规定时间内回收有效数据,采用稳健(Robust)统计进行分析并给出结论。结果在反馈结果的163家实验室中,16家实验室的检测结果为不满意,8家实验室的检测结果为可疑,139家实验室的检测结果为满意,满意率为85.3%。结论本次能力验证活动中,85.3%的满意率表明绝大部分实验室具备饮料中柠檬黄的检测能力。但依然存在部分实验室的评价结果为可疑或不满意的情况,应分析原因并进一步提高实验室的检测能力。     

Conditioning unfamiliar and familiar flavours to specific positive emotions

Emotions play an important role in determining food preferences and liking. We often speak of food as something that evokes emotions, such as comfort food. In two studies we investigated whether novel and familiar flavoured drinks could be conditioned to evoke specific positive emotions and whether this had a subsequent effect on liking of the drinks. In the first study, 167 participants consumed one of two novel flavoured drinks (one initially highly liked, one initially medium liked) for five consecutive days while watching film clips evoking either joy, contentment or no emotion in a between subjects design. On the test day, we measured whether the emotions from the film clips were transferred to the drink, i.e. that the drink (which has no active ingredients) on its own induced a joyful/activating or contented/relaxed response. Behavioural measures showed that the conditioned drinks successfully induced the distinct positive emotions. Further, the emotional associations impacted on the liking of the drink. Liking scores for identical stimuli were different based on which emotion the drinks were associated with. In the second study with 139 participants, the same paradigm was used with familiar flavours. No emotional conditioning effects were found. These results suggest that it is possible to induce specific positive emotions by flavour conditioning in the absence of active ingredients for novel but not for familiar flavours, confirming that existing associations cannot be easily erased by new conditioning.     

磁分散萃取-液相色谱法测定食品接触材料中 3种酚类物质迁移量

目的合成一种表面多孔结构的磁性微球,用于食品包装材料迁移物的吸附富集,实现高灵敏度检测痕量组分。方法采用一锅法合成羧基化磁性微球,再经自组装法制备磁性金属有机骨架复合材料,并以此作为萃取剂,建立磁分散萃取-高效液相色谱法分离分析聚碳酸酯(PC)水杯中酚类化合物迁移量的新方法。结果平均回收率为85.36%~95.47%,相对标准偏差(RSD,n=5)为1.28%~5.64%,检出限和定量限分别为1.24~2.14 ng/m L和4.15~7.12 ng/m L。结论该合成方法简便可行,其磁性复合微球吸附性能好。该萃取和检测方法具有操作简便快速、富集倍数较高、灵敏度和准确度较好的特点,适用于酚类化合物的分离分析。     

运动饮料及其功能性成分的研究进展

运动饮料是根据人体运动时的生理消耗特点进行配制的,可针对性地补充运动消耗的营养,保持并提高运动能力,缓解运动产生的疲劳。随着国际竞技体育的多元化发展及全面健身运动潮流的兴起,运动营养食品得到了长足的发展,运动饮料作为一种新型运动营养补充剂,成为新宠,拥有广阔的市场前景。因而科学研制运动饮料已成为研究热点。本文根据运动饮料的发展、应用原料的功能进行综述,对其未来发展方向进行展望,并提出一定的建议。     

苦菜沙棘复合饮料的研制

天然苦味饮料是当今软饮料中的一种新型产品,苦菜是加工苦味饮料的好原料。本试验对苦菜沙棘复合饮料的加工工艺和操作技术进行了研究,获得了最佳配方和加工工艺。     

食品中违禁色素种类及高通量检测技术进展

工业染料是食品中常见的违法添加色素,是食品中常见的非法添加物。本文根据工业染料的化学性质,将食品中易违法添加的近40种违禁色素分为酸性,中性和碱性,对它们的理化性质、易非法添加的食品种类、毒性危害与法规限制,以及多种禁用色素多重高通量分析测试方法的前处理、线性范围、检出限和回收率等方面做出综述,并分析了各种检测技术的优缺点和适用性。作者认为非食用色素检测技术将趋于利用液相色谱串联质谱的高通量筛选和利用免疫学或电化学的快速检测方向发展,检测方法将更快速、环保、低成本、高自动化程度,并会针对不同的检测需求制定相应的检测方法,分别满足实验室确认分析和现场快速筛查的需求。