The Application of NMR Spectroscopy and Chemometrics in Authentication of Spices

Spices and herbs are among the most commonly adulterated food types. This is because spices are widely used to process food. Spices not only enhance the flavor and taste of food, but they are also sources of numerous bioactive compounds that are significantly beneficial for health. The healing effects of spices are connected with their antimicrobial, anti-inflammatory and carminative properties. However, regular consumption of adulterated spices may cause fatal damage to our system because adulterants in most cases are unhealthy. For that reason, the appropriate analytical methods are necessary for quality assurance and to ensure the authenticity of spices. Spectroscopic methods are gaining interest as they are fast, require little or no sample preparation, and provide rich structural information. This review provides an overview of the application of NMR spectroscopy combined with chemometric analysis to determine the quality and adulteration of spices.     

A Novel and Reusable Electrochemical Genosensor for Detection of Beef Adulteration

This work describes the construction of a genosensor based on a graphite electrode modified with an reduced graphene oxide/poly(3-hidroxybenzoic acid) nanocomposite with an specific DNA oligonucleotide for detection of cattle mitochondrial DNA, in order to certify beef purity. Electrochemical and morphological analyses indicate that the genosensor allows duplex formation with the DNA of pure sample of beef lysate. The genosensor was selective, identifying up to 1 % (w/w) of pork in beef samples, showing good reproducibility and stability within six weeks of storage, and can be reused four times, being a great tool for the evaluation of beef purity, with application in the meat production and marketing chain.     

基于高效液相色谱-四极杆/静电场轨道阱高分辨率质谱的寡糖轮廓分析用于蜂蜜中淀粉糖浆的掺假鉴别研究

采用高效液相色谱-四极杆/静电场轨道阱高分辨率质谱(HPLC-Q/Orbitrap MS)建立了寡糖轮廓分析的方法。通过对纯天然蜂蜜和淀粉类糖浆中的麦芽三糖、麦芽四糖、麦芽五糖、麦芽六糖和麦芽七糖进行定性定量分析,发现淀粉类糖浆中含有未被酶解完全的微量麦芽类寡糖,且麦芽七糖在所有检测样本中干扰小,对结果的定量无影响,而其他寡糖类物质的定性和定量结果会存在干扰。最终选择麦芽七糖作为蜂蜜中掺入淀粉糖浆的典型标志物。在实际样品分析中,根据麦芽七糖的保留时间和离子对的相对丰度比可以定性判断蜂蜜中是否掺有淀粉糖浆;通过标准曲线法可以定量测定样液中麦芽七糖的含量。在20,50,100 mg/kg 3个加标水平下,麦芽七糖的平均回收率为75%~82%,相对标准偏差(RSD,n=5)为3.1%~6.7%,方法检出限为0.1μg/m L。应用该方法可在10 min内完成整个分析过程,且样品前处理简单,结果可靠,灵敏度高,可用于纯天然蜂蜜中掺入淀粉糖浆的快速确证和检测。     

Ba~1~-~1~.~5~yLa~ySn~xTi~1~-~xO~3固溶体的合成、结构与性能

用软化学合成方法,在100^oC以下制备了一系列Ba~1~-~1~.~5~yLa~ySn~xTi~1~-~xO~3固溶体纳米粉末,XRD物相分析和d间距-组成图证明,产品为完全互溶取代固溶体.TEM观察,粒子为均匀球形,平均粒径70nm.通过制陶实验,分别测定了该系列固溶体的室温介电常数,结果发现,用化学方法在BaTiO~3中掺入适量锡和镧,引起T~c降低,当x=0.2,y=0.08时,室温介电数高达28000,比BaTiO~3纯相提高20倍.     

LiNi0.8Co0.2-XMXO2的合成和电化学性能研究

锂离子电池手机、笔记本电脑、电动汽车技术、医疗仪器电源以及宇宙空间等领域。目前商品化锂离子电池正极活性材料主要是LiCoO2、LiNiO2、LiMn2O4,及其掺杂化合物。LiNiO2具有比容量高,功率大、价格适中等优点,但也存在合成困难,热稳定性差等问题,其实用化进程一直比较缓慢。     

LaSrCo_(0.9)B'_(0.1)O_4复合氧化物制备、氧化性能及表征

采用聚丙烯酰胺法制备了类钙钛矿LaSrCo0.9B'0.1O4系列复合氧化物(B'=Mn、Fe、Ni、Cu)和LaSrCoO4,并考察了对CO和C3H8催化氧化反应的活性,运用XRD、BET、TEM、TPD等方法对LaSrCo0.9Ni0.1O4、LaSrCoO4进行了表征.结果表明,LaSrCo0.9Ni0.1O4和LaSrCoO4都为四方K2NiF4型纳米材料.Ni的掺入提高了LaSrCoO4的催化活性、O的吸附量和晶格畸变率,降低了平均晶粒度.     

Sugar Profiling of Honeys for Authentication and Detection of Adulterants Using High-Performance Thin Layer Chromatography

Honey adulteration, where a range of sugar syrups is used to increase bulk volume, is a common problem that has significant negative impacts on the honey industry, both economically and from a consumer confidence perspective. This paper investigates High-Performance Thin Layer Chromatography (HPTLC) for the authentication and detection of sugar adulterants in honey. The sugar composition of various Australian honeys (Manuka, Jarrah, Marri, Karri, Peppermint and White Gum) was first determined to illustrate the variance depending on the floral origin. Two of the honeys (Manuka and Jarrah) were then artificially adulterated with six different sugar syrups (rice, corn, golden, treacle, glucose and maple syrup). The findings demonstrate that HPTLC sugar profiles, in combination with organic extract profiles, can easily detect the sugar adulterants. As major sugars found in honey, the quantification of fructose and glucose, and their concentration ratio can be used to authenticate the honeys. Quantifications of sucrose and maltose can be used to identify the type of syrup adulterant, in particular when used in combination with HPTLC fingerprinting of the organic honey extracts.     

单类分类方法结合光谱分析在食品真实性鉴别中的应用

近年来,假冒伪劣食品已日益成为广大消费者密切关注的问题,食品真实性评估是缓解这一问题、保护公众健康的有力手段。在仪器设备和样品处理的高要求下,现代检测技术通常需要大量时间和金钱的成本消耗,而如今食品掺假手段不断变换,花样日益翻新,使得这类检测技术存在一定的局限性。为促进食品安全质量监管的效率和水平提高,为监管工作提供有力的科学技术支撑和保障,需要寻求新型检测技术。光谱分析技术,以操作简单、快速无损的优势近年来被广泛应用,作为一种间接分析技术,结合数据统计学中的分类方法建立模型后更能有效进行真假鉴别。在分类方法中,由于现实生活中五花八门的掺假类型以及在真假样本数量差异大的情况下,常用的分类方法效果可能出现偏差。但单类分类方法(one-class classification)是一种只针对一类实例建模分析,以特定的置信水平固定目标样本类的边界,对新样本的类别进行判定的方法,利用这一特点能有效区分不同于真实样本的数据,大大减少了检测的工作量,在食品掺假检测应用领域有一定的发展潜力。对近年来模式识别中的分类方法——单类分类方法进行了综述。通过阐述光谱分析结合分类方法用于食品掺假检测的必要性,比...     

Durum wheat adulteration detection by NIR spectroscopy multivariate calibration

In the present work, we explored the possibility of using near-infrared spectroscopy in order to quantify the degree of adulteration of durum wheat flour with common bread wheat flour. The multivariate calibration techniques adopted to this aim were PLS and a wavelet-based calibration algorithm, recently developed by some of us, called WILMA. Both techniques provided satisfactory results, the percentage of adulterant present in the samples being quantified with an uncertainty lower than that associated to the Italian official method. In particular the WILMA algorithm, by performing feature selection, allowed the signal pretreatment to be avoided and obtaining more parsimonious models.     

Authentication of Iranian Saffron (Crocus sativus) Using Stable Isotopes δ13C and δ2H and Metabolites Quantification

Saffron is a very high value-added ingredient used in the food supplement market and contains a high level of safranal. Adding synthetic safranal to saffron, which is significantly cheaper, and falsifying the origin of saffron may represent recurrent fraud. Saffron from different countries was analyzed to determine the stable isotope ratios δ¹³C and δ²H from safranal by gas chromatography coupled with isotope-ratio mass spectrometry (GC-C/P-IRMS) and the concentration of saffron metabolites with ultra-high performance liquid chromatography coupled with diode array detector (UHPLC-DAD). The isotopic analysis highlighted a higher ratio of δ²H in synthetic safranal than in natural safranal; the mean values were 36‰ (+/− 40) and −210‰ (+/− 35), respectively. The δ¹³C between Iranian, Spanish and other saffron was significantly different and represents median values of −28.62‰, −30.12‰ and −30.70‰, respectively. Moreover, linear and quadratic discriminant analyses (LDA and QDA) were computed using the two isotope ratios of safranal and the saffron metabolites. A first QDA showed that trans-crocetin and the δ¹³C of safranal, picrocrocin, and crocin C3 concentrations clearly differentiated Iranian saffron from other origins. A second model identified δ¹³C, trans-crocetin, crocin C2, crocin C3, and picrocrocin as good predictors to discriminate saffron samples from Iran, Spain, or other origins, with a total ability score classification matrix of 100% and a prediction matrix of 82.5%. This combined approach may be a useful tool to authenticate the origin of unknown saffron.