稳定同位素技术在果汁中的应用

近年来,稳定同位素技术已发展成为解决食品掺假及产地溯源问题的一个强有力的手段.本文主要介绍了稳定同位素技术的基本原理,测试方法标准以及稳定同位素技术在果汁的真伪鉴别及产地溯源中的研究现状及实际应用.     

石斛中主要特征成分测定研究进展

石斛作为我国传统的中草药,具有较好的生理活性。石斛中主要的特征成分包括酚类、碱类和香豆素类化合物,对这些化合物的化学结构、检测方法、检测灵敏度及检测方法的精密度和准确度进行综述,为石斛的质量控制、产地溯源及真伪鉴别等提供技术支撑。     

数据融合策略在食品产地溯源中的应用进展

产地溯源技术可有效识别食品来源,在保护消费者权益和维护产品声誉方面具有重要作用。产地溯源常用的检测手段包括光谱、质谱、色谱和传感器技术等,但是对于化学组成较复杂的食品,单一的分析技术通常无法获得足够的化学信息,而数据融合策略可以通过对不同检测技术获取的数据进行处理及联合,获取更多的有用信息,提高在产地溯源过程中的鉴别效果。目前,数据融合策略已经广泛应用于食品产地溯源领域。本文介绍了包括光谱、质谱、色谱和传感器技术等产地溯源检测技术,总结了基于这些技术的数据融合策略在食品产地溯源中的应用现状,并对数据融合策略在食品产地溯源方面的发展前景进行了展望,以期为食品产地溯源的研究及发展提供参考。     

水产品溯源中的同位素技术研究进展

水产品质量参差不齐,养殖方式多种多样,产地来源也各不相同,普通消费者难以从外观和口感来鉴别其真实来源。近年来,同位素质谱技术被认为是最可靠、最常用的溯源手段。综述了同位素质谱技术及其联合脂肪酸组成和元素组成在水产品溯源中的应用研究进展,并对其发展趋势进行了展望。     

稳定同位素质谱技术在香精香料鉴别研究中的应用

稳定同位素质谱技术作为产地溯源和真伪鉴别的有效技术之一,近年来被越来越多的应用于食品研究工作中。本文简要介绍了稳定同位素质谱技术的基本原理和常用的稳定同位素分馏机理,对稳定同位素质谱技术在香精香料鉴别研究中的国内外进展进行了综述,并对该技术的发展进行了展望。旨在促进稳定同位素质谱技术在香精香料鉴别研究中的应用,推动稳定同位素数据库及鉴别技术体系的建立和完善。     

基于质谱的蛋白质组学技术在食品真伪鉴别及品质识别方面的应用

蛋白质组学作为后基因组时代的一个新研究方向,近几年发展迅速,目前已应用于多个领域,在食品品质检测和安全控制方面成为有力的研究工具。蛋白质组学为食品科学的相关研究打开了新思路,不仅可以鉴定蛋白质种类,还可进行蛋白质定量,为分析不同物种、产地、成熟阶段的食品蛋白质组分和含量提供了可能。蛋白质组学研究手段多样,质谱是常用技术之一。该文介绍了蛋白质组学的概念、分类、研究技术以及常见蛋白质数据库,综述了基于质谱的蛋白质组学技术在真伪鉴别和品质检测方面的应用,涉及海鲜、肉制品、奶制品、保健食品及高附加值食品等多种食品,并对蛋白质组学的发展进行了展望。     

稳定同位素法测定大豆水溶性蛋白质中碳、氮、氧、氢稳定同位素比值及其在产地溯源鉴定中的应用

利用元素分析-同位素比质谱仪(EA-IRMS)测定了来自美国、巴西、阿根廷和加拿大产的60份大豆样品中水溶性蛋白质的δ^(13)C、δ^(15)N、δ^(18)O和δ^(2)H值,采用OPLS-DA统计分析方法构建大豆产地溯源模型。大豆水溶性蛋白质δ^(13)C、δ^(15)N、δ^(18)O和δ^(2)H值分别为-24.675‰~-29.490‰,-1.595‰~2.537‰,15.749‰~25.127‰,-33.504‰~-118.697‰。比较PCA和OPLS-DA两种统计分析方法显示,OPLS-DA统计分析方法建立的大豆产地溯源鉴别模型识别准确率更高,δ^(15)N、δ^(2)H、δ^(18)O和δ^(13)C在溯源模型中对产地识别的贡献度VIP值分别为1.069,1.045,1.035,0.834。大豆水溶性蛋白质δ^(13)C、δ^(15)N、δ^(18)O和δ^(2)H产地溯源OPLS-DA模型可鉴别美国、加拿大、巴西和阿根廷四个国家生产的大豆样品,在此基础上构建美国与其他3个国家的两两产地识别模型,可准确鉴别美国产大豆,识别准确率为100%。该研究方法和所构建的模型可应用于美国、巴西、阿根廷和加拿大产大豆的产地溯源。     

利用DNA条码对农产品产地溯源研究——黑木耳产地分子溯源

以黑木耳为例,利用DNA条码(ITS条码)对采自5个不同产地的24份黑木耳样品进行了产地溯源的分子检测研究。实验结果表明ITS条码能清楚溯源分别采自东北和未知地1的10个黑木耳样品,但未能溯源分别采自湖北、四川和未知地2的14个黑木耳样品,可能是产自湖北、四川和未知地2的样品DNA突变率低,积累的突变低于ITS条码的分辨率。因此,对于地理标志农产品的分子溯源应扫描多种基因片段以获得更多的DNA突变位点,提高DNA条码对农产品产地的溯源灵敏度。     

基于矿物元素指纹图谱鉴定陈皮产地的方法研究

采用电感耦合等离子体质谱法测定了新会、广西、湖南3地42批陈皮样品中51种矿物元素的含量,运用方差分析和偏最小二乘法-判别分析（PLS-DA）研究了不同产地陈皮中矿物元素的差别,以筛选得到的9种元素为溯源指标,将不同数量级矿物元素含量进行分类和系数缩放后,构建了陈皮中矿物元素的指纹图谱,并基于各产地矿物元素含量的平均值构建了新会、广西、湖南产地陈皮中矿物元素的标准指纹图谱。通过采用SPSS20.0计算18批新会陈皮矿物元素指纹图谱与其标准指纹图谱的相似度,确定新会陈皮矿物元素指纹图谱的相似度阈值为0.941,基于此阈值建立了新会陈皮的鉴别模型。采用24批样品对所建立的鉴别模型进行准确性验证,正确率为91.6%。该方法操作简单直观,满足实验分析要求,可为陈皮的产地溯源提供参考。     

不同产地川党参微量元素的聚类分析

用原子吸收火焰法（FAAS）测定了28个不同产地和采收时间的川党参的7种微量元素,用DPS8．5版软件对测试结果进行聚类分析。结果显示,除重庆武隆县以外的川党参都非常接近,该法可简便地鉴别不同产地和采收时间的川党参真伪。     

Chromatography in authenticity and traceability tests of vegetable oils and dairy products: a review

The new applications of various chromatographic techniques such as gas-liquid chromatography, high-performance liquid chromatography and electrophoretic methods employed for the analysis in macro- and micro-components in vegetable oils and dairy products are compiled and critically evaluated. The employment of these methods for authenticity tests and traceability is discussed.     

龙井茶特征香气成分分析及种类判别

采用顶空固相微萃取(HS-SPME)和气相色谱-质谱(GC-MS)联用技术分析了39份龙井茶叶中的挥发性成分,结合质谱数据库与保留指数,从24份西湖核心区龙井茶中获得了200余种挥发性化合物,这些挥发性成分中主要含有醇类、酯类、酮类、杂环类等化合物,经筛选得到26种共有组分.并采用主成分分析法(PCA)对24份西湖核心区龙井茶和15份疑似龙井茶进行了有效区分.该方法适用于茶叶的品质鉴定、真假识别、产地溯源等方面的研究,也为其他产品的挥发性成分分析提供参考.     

Development of a multiplex DNA-based traceability tool for crop plant materials

The authenticity of food is of increasing importance for producers, retailers and consumers. All groups benefit from the correct labelling of the contents of food products. Producers and retailers want to guarantee the origin of their products and check for adulteration with cheaper or inferior ingredients. Consumers are also more demanding about the origin of their food for various socioeconomic reasons. In contrast to this increasing demand, correct labelling has become much more complex because of global transportation networks of raw materials and processed food products. Within the European integrated research project ‘Tracing the origin of food’ (TRACE), a DNA-based multiplex detection tool was developed—the padlock probe ligation and microarray detection (PPLMD) tool. In this paper, this method is extended to a 15-plex traceability tool with a focus on products of commercial importance such as the emmer wheat Farro della Garfagnana (FdG) and Basmati rice. The specificity of 14 plant-related padlock probes was determined and initially validated in mixtures comprising seven or nine plant species/varieties. One nucleotide difference in target sequence was sufficient for the distinction between the presence or absence of a specific target. At least 5% FdG or Basmati rice was detected in mixtures with cheaper bread wheat or non-fragrant rice, respectively. The results suggested that even lower levels of (un-)intentional adulteration could be detected. PPLMD has been shown to be a useful tool for the detection of fraudulent/intentional admixtures in premium foods and is ready for the monitoring of correct labelling of premium foods worldwide.     

Accreditation: worth the trouble?

 Since the late 1980s, much attention has been paid to the usefulness of ISO-9000 certification. At present more than 45000 companies and institutions worldwide have been granted an ISO-9000 certificate. In the field of quality assurance, however, the ISO-9000 series does not completely cover the aspect of traceability. Demonstrable traceability is a particular problem in quality assurance of products by chemical analysis. In this paper realisation of demonstrable traceability is discussed, using the field of gas analysis as an example. Attention is focused on the usefulness of accreditation for laboratories performing quality assurance analyses. The basic question is asked whether and, if so, when accreditation is worth the trouble in cases where demonstrable traceability is required. Received: 15 February 1996 Accepted: 6 March 1996     

Identification of Ensis siliqua samples and establishment of the catch area using a species-specific microsatellite marker

European Council Regulation 104/2000 states that fishery products must be labeled to indicate commercial designation of species, the production method, and the catch area. Therefore, traceability of seafood implies knowledge of the species offered to retail and their origin. Ensis siliqua is a bivalve intensively fished in Europe and sold in fresh and canned forms. Although several published methods clearly differentiate Ensis genus species, none of those assess the origin of the commercial samples. In the present study, a microsatellite marker (Esi-UDC3055F) was developed to establish the catch area of E. siliqua samples. Amplification yielded a fragment of 275 or 302 base pairs, depending on whether they were Iberian or Irish populations. The usefulness of this method was also assessed in commercial samples. The results of this study provide a reliable methodology for the identification of catch area in European E. siliqua commercial samples. The coupling of this methodology with existing techniques for razor clam species identification provides a powerful tool for traceability and labeling enforcement.     

Study of organic honey from the Northeast Portugal

Concerns about traces of numerous toxic substances and authenticity have prompted consumer demand for honey that is certified as organic, based on strict ecological, natural principles and traceability. The present study aims to characterize organic honey samples (n = 73) from Northeast Portugal, with respect to floral nectar origin, physicochemical parameters and microbial safety. The phenols and flavonoids contents, often referred to as responsible for honey's bioactive properties, were also assessed. All organic honey samples were classified as monofloral lavender (Lavandula sp.), exceeded in quality the international physicochemical standards and showed low microbiological counts (yeast, moulds and aerobic mesophiles), with negative results in respect to fecal coliforms, Salmonella and sulphite-reducing Clostridium spp. Correlation of the palynological, physicochemical and microbiological results is necessary to check the authenticity, quality and sanitation of honey. Although not required by international legislation, results of those assessments provide a complete outlook and elucidation of the organic honey's properties, which could promote its valorisation.     

LC/MS study of the UV filter hexyl 2‐[4‐(diethylamino)‐2‐hydroxybenzoyl]‐benzoate (DHHB) aquatic chlorination with sodium hypochlorite

The fate of modern personal care products in the environment is becoming a matter of increasing concern because of the growing production and assortment of these compounds. More and more chemicals of this class are treated as emerging contaminants. Transformation of commercially available products in the environment may result in the formation of a wide array of their metabolites. Personal care products in swimming pools and in drinking water reservoirs may undergo oxidation or chlorination. There is much data on the formation of more toxic metabolites from original low toxicity commercial products. Therefore, reliable identification of all possible transformation products and a thorough study of their physicochemical and biological properties are of high priority. The present study deals with the identification of the products of the aquatic chlorination of the hexyl 2‐[4‐(diethylamino)‐2‐hydroxybenzoyl]‐benzoate ultraviolet filter. High‐performance liquid chromatography/mass spectrometry (HPLC/MS) and HPLC/MS/MS with accurate mass measurements were used for this purpose. As a result, three chlorinated transformation products were identified. Copyright © 2013 John Wiley & Sons, Ltd.     

Herkunft und Authentizität von Lebensmitteln: Stabilisotopenanalytik

The correlations between isotope ratios in water, organic mass, and trace elements of food and beverages, and the circumstances and sites of their origin and production are outlined, and the methods of mass spectrometric isotope ratio determination and the positional ²H analysis by quantitative NMR measurement are explained. In context with the application of these methods for origin and authenticity investigations of food, examples are given for the proof of watering or sugar addition to wine and fruit juices and methods for the identification of nondeclared additions of L‐malic and Lascorbic acids are described. The possibilities of multielement isotope ratio analysis for the identification of origin of animal products (eggs, milk products, meat) and methods for the discriminations between natural and nature identical aroma compounds are outlined. Finally, the possibilities of isotope ratio measurements for the discrimination between plant and animal food from conventional and organic production are discussed.     

Pyrolysis and soft ionization mass spectrometry of aquatic/terrestrial humic substances and soils

The rapid, reproducible, chemical characterization of complex environmental materials such as plants, humic substances and whole soil can be performed by controlled thermal degradation. Except for drying and milling no pre-treatment of the samples is required. Biomacromolecular cleavage during a short degradation step directly in the ion source of a mass spectrometer results in the production of high-mass chemical subunits. Short reaction times and small amounts of sample favour the generation of large, thermal fragments, i.e., chemical building blocks, which can be identified and correlated with the structure of the polymeric biomaterials investigated. The principal aim is to monitor the primary, thermal fragmentation by high molecular ion intensities of the pyrolyzates and to avoid consecutive, mass spectrometric fragmentation as far as possible.For the detection and identification of the pyrolysis (Py) products, a combination with time-/temperature-controlled mass spectrometry (MS) is used. Typical heating rates are 0.2–10°C/s and the temperature range is 50–800°C. Soft ionization techniques such as field ionization (FI), field desorption, chemical ionization (CI) and, to some extent, fast atom bombardment are employed in the positive and negative modes. The results of direct Py-MS are supported by high-resolution mass measurements using electric or photographic detection and Curie-point pyrolysis in combination with gas chromatography-electron ionization/FI/CIMS and library searches for the identification of the pyrolysis products.Fingerprinting and time-resolved Py-MS of aquatic and terrestrial humic substances are reported. The methodology for the investigations of dynamic processes during the volatilization and thermal decomposition of these complex biomaterials is illustrated. Weight loss curves and the temperature function of accurate molecular weight averages for aquatic fulvic and humic acid are derived from the Py-FIMS data. Initial results on the differentiation of soil horizons in a moder profile by Py-FIMS and pattern recognition are presented. In particular, the chemometric evaluation appears promising for future Py-MS studies of humic substances and whole soils, but also for fossil fuels, synthetic polymers and food. In an integrated approach, the linking of conventional chemical and spectroscopic data with the high-mass signals in pyrolysis-mass spectra will be the focus of forthcoming work. Preliminary results for combining wet-chemical data with those of ¹³C nuclear magnetic resonance, Fourier transform infrared and electron spin resonance spectroscopy are put forward in this survey. Finally, initial results of pilot studies to detect biocides such as atrazine directly in soils using Py-FIMS are demonstrated.     

Multielemental characterization of honey using inductively coupled plasma mass spectrometry fused with chemometrics

Honey is considered a desirable ingredient in a range of different foodstuffs because of its nutrient and therapeutic effect. The honey characteristics mainly depend on the type of vegetation visited by the bees and the climatic conditions in which the plants are growing. Therefore, the purity, floral and geographical origin and authenticity are important factors influencing the overall perception of honey and honey‐based products in terms of quality and price. An important parameter in this picture is the elemental composition of honey because it can be linked with the floral type of honey, floral plant density and the botanical origin of nectar and pollens. In this work, the concentration range variation of 18 elements (Al, As, Ba, Ca, Cd, Co, Cr, Cu, Mg, Mn, Na, Ni, K, Pb, Sr, Ti, V and Zn) was investigated in four varieties of honey (linden, acacia, rape, and sunflower) originating from Romania, because the elemental profile of honey may give important information to differentiate its geographical and varietal origin for authenticity purpose. All the determinations were carried out by inductively coupled plasma quadrupole mass spectrometry (ICP‐Q‐MS). The most abundant minerals decreased in the following order: K > Ca > Mg > Na, having the mean values of 248.70, 59.97, 20.54 and 11.92 mg kg^?1, respectively. The mineral content marks the differences in honey samples from different botanical origin and can be used as a tool for authentication purposes and also extends its applicability to assess the traceability of honey. Analysis of variance showed the preliminary relationships between the elements and samples. Further, the discrimination between different studied honey samples was achieved by principal component analysis (PCA). The multivariate analysis of the data allowed us to separate the honey samples into distinct groups according to their macroelement and microelement composition, emphasizing the origin of variation of element concentrations by honey type. Therefore, this approach might be potentially useful for the control of honey quality, origin or authenticity, and even to use the honey as environmental tracer.