An Improved Approach to Identify Irradiated Spices Using Electronic Nose,FTIR, and EPR Spectroscopy

Changes in cumin and chili powder from India resulting from electron‐beam irradiation were investigated using 3 analytical methods: electronic nose (E‐nose), Fourier transform infrared (FTIR) spectroscopy, and electron paramagnetic resonance (EPR) spectroscopy. The spices had been exposed to 6 to 14 kGy doses recommended for microbial decontamination. E‐nose measured a clear difference in flavor patterns of the irradiated spices in comparison with the nonirradiated samples. Principal component analysis further showed a dose‐dependent variation. FTIR spectra of the samples showed strong absorption bands at 3425, 3007 to 2854, and 1746 cm^?1. However, both nonirradiated and irradiated spice samples had comparable patterns without any noteworthy changes in functional groups. EPR spectroscopy of the irradiated samples showed a radiation‐specific triplet signal at g = 2.006 with a hyper‐fine coupling constant of 3 mT confirming the results obtained with the E‐nose technique. Thus, E‐nose was found to be a potential tool to identify irradiated spices.     

A new high-throughput screening method to determine multiple dyes in herbs and spices

The unauthorised addition of colours to herbs and spices is a recurrent issue affecting food business operators. Such a practice aims at improving food visual attractiveness, masking poor product quality, and/or compensating for natural colour variation with the ultimate goal to increase profits. To detect this fraud, a new LC–MS/MS method was developed for screening 58 dyes in both herbs and spices. This extended list of targets was established based on requirements from international spices organisations, past issues identified by web scouting and by notifications from the European Rapid Alert System for Food and Feed (RASFF). The method is intended to quickly detect fraudulent addition of dyes with Screening Target Concentrations ranging from 0.1 to 2.5 mg/kg. Validation was performed according to the European Community Reference Laboratories Residues Guidelines 20/1/2010. False positive and false negative rates were below 5% for all analytes and applicability of the method was further demonstrated by analysing 117 samples collected worldwide. None of the surveyed dyes was found in herbs (n = 28, 16 varieties) whereas 6% of spice samples (n = 89, 21 varieties) was found contaminated with one or two dyes at levels ranging from 0.12 to 255 mg/kg. Four out of the nine detected compounds have never been reported in the RASFF, thus demonstrating the usefulness of this analytical approach.     

New Opportunities of the Application of Natural Herb and Spice Extracts in Plant Oils: Application of Electron Paramagnetic Resonance in Examining the Oxidative Stability

The aim of this study was to establish the applicability of natural water-ethanol extracts of herbs and spices in increasing the oxidative stability of plant oils and in the production of novel food. Different concentrations (0, 100, 300, 500, and 700 ppm) of spice extracts and butylated hydroxyanisole (BHA) (100 ppm) were added to the studied oils. The antioxidant activity of spice extracts was determined with electron paramagnetic resonance (EPR) spectroscopy using 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical assay. The study showed that the extracts significantly increased the oxidative stability of the examined oils when compared to one of the strongest synthetic antioxidants-BHA. The applied simple production technology and addition of herb and spice extracts to plant oils enabled enhancement of their oxidative stability. The extracts are an alternative to the oils aromatized with an addition of fresh herbs, spices, and vegetables because it did not generate additional flavors thus enabling the maintenance of the characteristic ones. Moreover, it will increase the intake of natural substances in human diet, which are known to possess anticarcinogenic properties.     

Identification of irradiated foods by the thermoluminescence of mineral contamination

This investigation assessed the radiation-induced thermoluminescence (TL) of food minerals for identifying irradiated foods. Mineral contamination, rather than the inherent mineral content, of foods was studied. Positive identification of foods given 1-10-kGy doses depends on the contents and composition of the mineral contamination and the time span between irradiation and TL analysis. All 20 irradiated spice and herb samples could be identified without comparing them with unirradiated material. Three out of 60 lots of spices and herbs examined so far were so pure that the mineral contents were too low to allow TL analysis. If the soil where potatoes are grown contains feldspars, sprout inhibition treatment with 100-200-Gy doses can also be detected for up to one year, using the 90-250 degrees C low-temperature part of the TL spectrum for evaluation.     

Identification of irradiated spices with thermo-and chemiluminescence measurements

Thermoluminescence and chemiluminescence intensities of twenty-nine different spices were measured to determine whether the techniques could be used to detect if spices had been irradiated (10 kGy) and stored after irradiation. In each case it was possible to identify radiation treatment with 10 kGy by at least one of the two methods, if irradiation occurred 2–3 weeks prior to the examination. The luminescence effect from radiation treatment differs from spice to spice. Intensity increases in samples treated with 10 kGy vary between 1 (no effect) and about 1000 times compared with untreated samples. Thermoluminescence proved to be more useful than chemiluminescence, as with most spices radiation treatment could be identified after longer periods of time. A combined or simultaneous use of both techniques assures a rapid identification of radiation treatment in most of the examined spices. With the exception of garlic, onions, white and black pepper, the irradiated spices can be identified more than 6 months after irradiation. Some, curcuma, juniper berries, basil, chillis, paprika and celery, show increased luminescence intensities for a year or longer after irradiation.     

Evaluation of a microbiological method for detection of irradiation of spices

The suitability of a microbiological method, a combination of the direct epifluorescent filter technique (DEFT) and the total aerobic plate count (APC), for the detection of irradiation of spices was evaluated. The evaluation was carried out using different kinds of spices including peppers, paprika, cardamom, cinnamon, ginger; herbs such as thyme, marjoram, basil, and oregano; and garlic powder. Ground spices were tested as well as cut and whole spice samples. Samples were analysed before and after gamma-irradiation mainly with doses of 5 and 10 kGy. Two different methods (centrifugation, filtration) for sample pretreatment were compared. Differences between the DEFT count and the APC with doses of 5 and 10 kGy varied between 3.9 and 6.8 and between 5.7 and 7.5 log units, respectively. The duration of storage after irradiation had no effect on the microbiological results. When applied to fumigated samples, the method might cause confusion in the absence of chemical analyses. The results of the analyses of samples treated by an unknown process indicated that the method could, in fact, detect irradiated samples, although it could not differentiate between irradiated and heat-treated samples.     

The Effect of Irradiation and Heat Treatment on Composition and Antioxidant Properties of Culinary Herbs and Spices — A Review

Besides the positive effects, γ-irradiation and heat treatment of foods usually lead to changes in their structure or composition, thus influencing their quality. In view of the fact that herbs and spices are important source of antioxidants in a human diet, any kind of treatment can have an impact on their antioxidant status, as well. In this contribution, we review the effects of γ-radiation and heat treatment on some constituents and antioxidant properties of culinary herbs and spices. Both methods of treatment result in some common qualitative changes in herbs and spices, mostly in the content of polyphenols or volatile components. The results of antioxidant testing assays are sometimes contradictory in observed effect or trends, in dependence on the manner of treatment and character of spice matrix. Based on this review, the effects of γ-radiation or heat processing on antioxidants, or the vitamin content in herbs and spices is still lacking, which makes the direct assessment of the effect of treatment on the antioxidant status of herbs and spices practically impossible. However, the changes in composition that have been observed to date suggest that they have only a small effect on the behavior of herbs and spices in a real food matrix.     

Electron spin resonance spectroscopy as probes for spices. Detection of treatment with ionizing radiation]

Detection of irradiated spices by electron spin resonance (ESR) measurements was not successful in the past because a central line of unknown origin was detected in the ESR-spectra of both irradiated and unirradiated samples. Identification of irradiated samples by measuring the increase of intensity of this signal after irradiation is limited because the signal intensity decreases over a period of some weeks of storage and reaches the range of unirradiated samples. By changing the measurement conditions (low microwave power) we could detect two additional lines on both sides of the main signal. This line pair appears only in the spectra of irradiated spices. A similar line pair was found in the spectra of irradiated nutshells and possibly derives from cellulose radicals in the sample. For some spices, especially paprika, the identification of irradiated samples by detecting these additional lines was possible even after relatively long periods of storage.     

Sterilization of Ground Prepacked Indian Spices by Gamma Irradiation

Prepacked ground Indian spices which included pepper. turmeric, chilli, and coriander were found to be heavily contaminated with bacteria and molds. The total bacterial counts ranged between 10⁵–10⁷. whereas total fungal counts ranged between 10²–10⁶. Red chilli was found to be the most contaminated spice. The bacterial population consisted mainly of spores. A dose of 10 kGy was found to be effective in destroying these microbes in prepacked spices without affecting their quality attributes. To eliminate mold contamination a dose of 5 kGy was sufficient. During a six-month storage study of irradiated and unirradiated spices, the irradiated spices were found to retain their quality.     

Spices and herbs as source of Salmonella-related foodborne diseases

Salmonella is a leading cause of foodborne diseases and the role of ready-to-eat products including plant-derived food is increasingly recognized. The present survey reviewed recent literature on Salmonella-related outbreaks caused by spices and herbs and on the occurrence of Salmonella in these food matrices. Spices and herbs contaminated with Salmonella were responsible for a variety of foodborne outbreaks in Europe and North America. Identified serovars did often not belong to those predominating in human illness. Moreover, in different survey studies, Salmonella belonging to a broad diversity of serovars were found in a variety of spices and herbs. The proportion of Salmonella-positive samples ranged from 0% to 8.4%, albeit detection rates were rather low in most studies. Higher prevalence rates were often obtained with regard to a specific spice or herb type. Due to high desiccation tolerance, Salmonella can survive for an extended period of time in spices and dried herbs. Thus, by the use of untreated spices and herbs for production of foods not subjected to a heat treatment or for seasoning of ready-to-eat products, Salmonella might be introduced and in this way might pose a threat to consumers.     

食用植物油掺假鉴别方法研究进展

阐述了食用植物油掺伪的现状,综述了理化方法、色谱法、核磁共振波谱法、红外光谱法、拉曼光谱法的检测原理,以及在食用植物油掺假鉴别中的研究进展.着重介绍了应用最广泛的色谱法,它主要通过对脂肪酸、甾醇、生育酚等物质的测定来进行掺伪鉴别.同时,对核磁共振波谱法、红外光谱法、拉曼光谱法在油脂掺伪检测中的初步应用进行了归纳.对掺伪检测技术的研究方向进行了展望.     

天然植物香料在食品中的利用现状

介绍了天然植物香料的品种和性质，重点阐述了植物香料的抑臭赋香作用，抗氧化作用，抑菌作用及其医药疗效作用。最后概括了植物香料工业的发展趋势。     

Natural occurrence of fumonisins and ochratoxin A in some herbs and spices commercialized in Poland analyzed by UPLC–MS/MS method

Unsanitary conditions during harvesting, drying, packing and storage stages in production and processing of spices and herbs could introduce mycotoxin contamination. The occurrence of ochratoxin A and fumonisins in popular spices and herbs was studied, using liquid chromatography-electrospray-mass spectrometry. Apart from mycotoxins, ergosterol as a factor indicating fungal development was also analysed. A total of 79 different samples commercialized in Poland were randomly purchased from popular markets were tested for mycotoxins. The frequency of samples with fumonisins was lower (31%) than ochratoxin A (49%). Free from mycotoxins were samples of bay leaf and white mustard. ERG content – in spice samples with high concentration level of mycotoxins – was also significantly higher than in samples with little to no mycotoxins.     

Development and application of Fourier transform infrared spectroscopy for detection of milk adulteration in practice

Fourier transform infrared (FT‐IR) spectroscopy is widely applied for routine milk analysis. More recently, it has been used to detect a range of specific milk adulterants. Here, we show that the simultaneous use of targeted and untargeted models applied to FT‐IR spectra for detecting potential milk adulterants across relevant concentration ranges is an effective strategy. Using an appropriate validation strategy, limits of detection, sensitivity and specificity are determined for specific adulterants giving a useful guide to how these models would work in a practical situation. Finally, theoretical limits of detection of a range of potential adulterants are listed.     

Nontargeted,Rapid Screening of Extra Virgin Olive Oil Products for Authenticity Using Near‐Infrared Spectroscopy in Combination with Conformity Index and Multivariate Statistical Analyses

A rapid tool for evaluating authenticity was developed and applied to the screening of extra virgin olive oil (EVOO) retail products by using Fourier‐transform near infrared (FT‐NIR) spectroscopy in combination with univariate and multivariate data analysis methods. Using disposable glass tubes, spectra for 62 reference EVOO, 10 edible oil adulterants, 20 blends consisting of EVOO spiked with adulterants, 88 retail EVOO products and other test samples were rapidly measured in the transmission mode without any sample preparation. The univariate conformity index (CI) and the multivariate supervised soft independent modeling of class analogy (SIMCA) classification tool were used to analyze the various olive oil products which were tested for authenticity against a library of reference EVOO. Better discrimination between the authentic EVOO and some commercial EVOO products was observed with SIMCA than with CI analysis. Approximately 61% of all EVOO commercial products were flagged by SIMCA analysis, suggesting that further analysis be performed to identify quality issues and/or potential adulterants. Due to its simplicity and speed, FT‐NIR spectroscopy in combination with multivariate data analysis can be used as a complementary tool to conventional official methods of analysis to rapidly flag EVOO products that may not belong to the class of authentic EVOO.     

Electron paramagnetic resonance detection of Mexican irradiated spices

Four different spices produced in Mexico, namely black pepper, two kinds of chilli and oregano, were studied by electron paramagnetic resonance (EPR) technique for detection purposes. In all the non‐irradiated spices we tested, the same single line signal at g = 2.0041 (native signal) was registered. Irradiation induced at least two EPR signals overlapping the native signal: an intense singlet and, with the exclusion of oregano, a weak triplet with hyperfine splitting of 3 mT due to cellulose free radicals. The recombination time of the free radicals produced by irradiation was short compared with the shelf‐life of the spices, thus limiting the application of the EPR technique for detection. To extend the time when these products may be identified as irradiated, the method proposed by Yordanov and Gancheva (Appl Radiat Isot 2000; 52 :195) was applied to the spices, but with no success. Thermoluminescence tests provided correct results for all the spices, even 2 years after irradiation.     

Evaluation of Antioxidant Effects and Sensory Attributes of Chinese 5-Spice Ingredients in Cooked Ground Beef

ABSTRACT This study determined antioxidant and sensory characteristics of cinnamon, cloves, fennel, pepper, and star anise (Chinese 5‐spice ingredients) in cooked ground beef. Total aerobic plate counts were also measured. Mean thiobarbituric acid (TBA) values were high (3.4 ppm) for control cooked ground beef samples. With 1% use level, all spice treatments had lower pooled mean TBA values than controls. At the lowest use level of 0.1% of meat weight, all spices except pepper had lower TBA values than controls. Treatments with 0.1% cloves had lower (P < 0.05) TBA values than 0.1% levels of other individual spices. Star anise, fennel, pepper, and cinnamon samples at 0.5% use level had lower mean TBA values than controls, but not different from 1.0% levels, respectively. Thus, the lowest effective spice level for cloves was 0.1% and 0.5% for the other spices. There was a high correlation (P < 0.01) between TBA values and panel scores for rancid odor and flavor (0.83 and 0.78, respectively). Spice flavor was inversely correlated (P < 0.01) with rancid odor and flavor (‐0.57 and ‐0.61, respectively). The 5‐spice blends did not affect microbial load of cooked samples compared with controls. In conclusion, all spices and blends had a dual effect, reducing rancid odor/flavor and imparting a distinctive flavor to cooked ground beef.     

EFFECT OF SPICES ON GROWTH AND SURVIVAL OF SALMONELLA TYPHIMURIUM DT 104 IN GROUND BEEF STORED AT 4 AND 8C

Few studies have addressed the use of spices against pathogens associated with meat. The effects of garlic, ginger and turmeric were evaluated against Salmonella Typhimurium DT 104 that were inoculated either in spice paste or in buffered peptone water (BPW) or in heat‐treated ground beef and stored at 4 and 8C for 10 days. Data from the spice pastes study showed a decrease in Salmonella Typhimurium DT 104 counts, and the greatest reduction (3.39 log) was observed in garlic paste stored at 4C. Garlic in BPW data showed a reduction of 1.5 and 1.0 log in Salmonella Typhimurium counts at 4 and 8C, respectively. Ground beef stored at 4C showed no growth or a slight reduction in growth in samples with spice, while all samples at 8C showed an increase in Salmonella Typhimurium counts. Results show that the spices inhibit or inactivate Salmonella Typhimurium DT 104 when they are in direct contact. However, when spices are added to a complex food system such as ground beef, the inhibitory activity of these spices considerably decreases.     

Culinary herbs inhibit lipid oxidation in raw and cooked minced meat patties during storage

The effect of dried spices and the ethanol extract of those spices was studied on the stability of fresh chicken minced meat, and fresh and cooked pork patties pretreated with NaCl during refrigerated and frozen storage. The antioxidant activities of the spices were measured by thiobarbituric acid reactive substances (TBARS) and peroxide value (POV) in meat samples. The lipid oxidation was effectively inhibited in the chicken meat treated with several dry spices diminishing the TBARS to a range of 32% and 83% of those found in the control samples in frozen stored meat for 6 months. Marjoram, wild marjoram and caraway were the most effective dry spices. Ethanolic extracts of the same spices were more potent as antioxidants by lowering the concentration of the TBARS to a range of 20–27% of those found in the control samples. Addition of sodium salt to the minced pork resulted very high concentrations of the oxidation products originated from the polyunsaturated fatty acids. The treatment with ethanolic extract of spices (sage, basil, thyme and ginger) significantly inhibited the lipid peroxidation in refrigerated and chilled pork patties pretreated with NaCl by reducing both POV and TBARS. Heat treatment with microwaves produced significantly elevated levels of both lipid peroxides and TBARS, but the amount of these oxidation products was less than 10% in spice‐treated salted meat samples compared to that in untreated ones. Lipid peroxidation also grew continuously during the storage period at −18°C in raw and cooked samples. Ethanolic extracts of spices had a very strong antioxidative effect inhibiting lipid peroxidation in heat‐treated meat products during frozen storage. The highest antioxidant activity was observed in the case of ginger. High correlation coefficients were found between TBARS and POV both in raw and cooked pork patties (0.86, 0.91, respectively) during frozen storage. It is supposed that these compounds originated from the polyunsaturated fatty acids during oxidation processes but at different stages. Utilization of spices, spice mixtures or spice extracts in semi‐prepared meat products intended to be frozen for up to 6 months or more before consumption is proved to be advantageous in regard of shelf life of the food, as well as of human health, because of the beneficial effect of spices in inhibition of lipid peroxidation during heat treatment and chilling storage. © 1999 Society of Chemical Industry     

Recalls of spices due to bacterial contamination monitored by the U.S. Food and Drug Administration: the predominance of Salmonellae

From 1980 to 2000, the annual per capita consumption of spices in the United States increased by 60% (from 1.0 to 1.6 kg per person per year). Although spices are known to harbor various molds, fungi, and bacteria, relatively few reports have documented this group of foods as the cause of human illness. In recent years, however, the U.S. Food and Drug Administration (FDA) has noted an increased number of recalls of dried spices due to bacterial contamination. Accordingly, we reviewed spice recalls that took place in the United States from fiscal years 1970 to 2003. During the study period, the FDA monitored 21 recalls involving 12 spice types contaminated with bacterial pathogens; in all but one instance, the recalled spices contained Salmonella. Paprika was the spice most often involved in the recalls. A wide variety of countries were the source of the recalled spices. Using data from the Centers for Disease Control and Prevention National Salmonella Surveillance System, we were unable to discern any increases in the reported incidence of laboratory-confirmed salmonellosis in states that received spices contaminated with selected rare Salmonella serotypes. A variety of effective methods exist to disinfect spices, procedures that have attained increased importance given the frequent use of spices in ready-to-eat foods and the potential for contaminated spices to cause widespread outbreaks.