Determination of Milk Fat Adulteration with Vegetable Oils and Animal Fats by Gas Chromatographic Analysis

This study assessed the potential application of gas chromatography (GC) in detecting milk fat (MF) adulteration with vegetable oils and animal fats and of characterizing samples by fat source. One hundred percent pure MF was adulterated with different vegetable oils and animal fats at various concentrations (0%, 10%, 30%, 50%, 70%, and 90%). GC was used to obtain the fatty acid (FA) profiles, triacylglycerol (TG) contents, and cholesterol contents. The pure MF and the adulterated MF samples were discriminated based on the total concentrations of saturated FAs and on the 2 major FAs (oleic acid [C18:1n9c] and linoleic acid [C18:2n6c], TGs [C52 and C54], and cholesterol contents using statistical analysis to compared difference. These bio‐markers enabled the detection of as low as 10% adulteration of non‐MF into 100% pure MF. The study demonstrated the high potential of GC to rapidly detect MF adulteration with vegetable and animal fats, and discriminate among commercial butter and milk products according to the fat source. These data can be potentially useful in detecting foreign fats in these butter products. Furthermore, it is important to consider that several individual samples should be analyzed before coming to a conclusion about MF authenticity.     

Bovine milk powder adulteration with vegetable oils or fats revealed by MALDI-QTOF MS

Matrix-assisted laser desorption/ionisation-quadrupole time of flight mass spectrometry (MALDI-QTOF MS) allowed detection of bovine milk powder adulteration with vegetable oils or fats with high speed and reliability, requiring little sample preparation (n-hexane extraction) and no prior separation procedures. This technique was also able to identify the adulterated employed in this fraud. Hydrogenated soybean oil addition in bovine milk powder sample generate a similar TAG profile to that observed on adulterated milk samples apprehended by the Brazilian Federal Police. In this sense, a robust method for high throughput forensic screening of milk powder adulteration by exogenous oils and fats is showed.     

Distinguishing lard from other animal fats in admixtures of some vegetable oils using liquid chromatographic data coupled with multivariate data analysis

Detection of animal fat adulterants in vegetable oils is of great importance from commercial and health perspectives. Distinguishable identification of lard contamination in some vegetable oils has been attempted in this study. Vegetable oils, namely palm oil (PO), palm kernel oil (PKO), and canola oil (CLO), were spiked with different proportions of animal fats, such as lard (GLD), beef tallow (BT), and chicken fat (CF). High-performance liquid chromatographic (HPLC) analyses were performed to monitor the triacylglycerol (TAG) compositional changes in the oil samples before and after adulteration. The results showed that qualitative determination of lard contamination in PKO was possible by a visual comparison of TAG profiles of PKO adulterated with different animal fats with those of the animal fats. This approach was not useful for PO and CLO. However, by subjecting liquid chromatographic data to multivariate procedures, distinguishable grouping of lard-contaminated samples was achieved for all three oils.     

Apparent solidification time test for detection of foreign oils and fats adulterated in clarified milk fat, as affected by season and storage

An apparent solidification time (AST) test was developed for the detection of foreign fats and oils in milk fat. AST values at 18°C for buffalo and cow milk fats ranged from 2 min 30 s to 2 min 48 s and 2 min 56 s to 3 min 26 s, while for pig body fat, goat body fat and hydrogenated vegetable oils, AST values were 1 min 30 s, 0 min 40 s and 1 min 50 s, respectively. Vegetable oils yielded no AST values, suggesting that adulteration can be detected using the AST method in the case of some but not all possible adulterants.     

Effectiveness of determinations of fatty acids and triglycerides for the detection of adulteration of olive oils with vegetable oils

This paper investigates the effectiveness of the determinations of fatty acids and triglycerides in the detection of adulteration of olive oil with certain vegetable oils. Detection of adulteration up to the level of 5% was possible. The use of the established limits of fatty acid contents could detect the adulteration of olive oil with the six of the investigated vegetable oils. The established limits of the ΔECN42 could be used to detect the adulteration of olive oil with the nine of the examined vegetable oils. Certain other parameters, based on differences of triglyceride and fatty acid compositions between olive oil and vegetable oils, could be used as discriminating factors between the olive oil and eight of the examined vegetable oils. However, no single known parameter could detect the presence of hazelnut and almond oils in olive oil, in percentages lower than or equal to 5%.     

Fatty Acid Composition Including Trans‐Fatty Acids in Edible Oils and Fats: Probable Intake in Indian Population

Abstract: The susceptibility of trans‐fat to the human health risk prompted the Food and Agriculture Organization (FAO) and World Health Organization (WHO) to prepare regulations or compulsory claims for trans‐fatty acids (TFA) in edible oils and fats. In this study, analysis of fatty acid composition and TFA content in edible oils and fats along with the possible intake of trans‐fat in Indian population was carried out. The analysis was carried out as per the Assn. of Official Analytical Chemists (AOAC) methodology and the results were statistically analyzed. The average TFA content in nonrefined mustard and refined soybean oils exceeded by 1.16‐ to 1.64‐fold as compared to the Denmark limit of 2% TFA in fats and oils destined for human consumption. In branded/nonbranded butter and butter oil samples, average TFA limit exceeded by 4.2‐ to 9.5‐fold whereas hydrogenated vegetable oil (HVO) samples exceeded the limit by 9.8‐fold, when compared to Denmark standards. The probable TFA intake per day through different oils in Indian population were found to be less than WHO recommendation. However Punjab having highest consumption of HVO (–15 g/d) showed 1.09‐fold higher TFA intake than the WHO recommendation, which is alarming and may be one of the factors for high cardiovascular disease mortality rate that needs further elucidation. Thus there is a need to prescribe TFA limit for edible oil, butter, and butter oil in India and to reduce the already proposed TFA levels in HVO to safeguard the health of consumers. Practical Application: The probable daily intake of trans‐fatty acid (TFA) especially through hydrogenated vegetable oil (HVO) was assessed. In absence of any specification for TFA and fatty acid composition for edible oils, butter, and butter samples, a pressing need was felt to prescribe TFA limit in India. The study indicates that TFA intake through HVO consumption is higher in States like Punjab than the recommended daily intake prescribed by WHO. Hence, strategies should be adopted to either decrease the consumption of HVO or to modify the industrial processing method of HVO with less content of TFA to safeguard the health of consumers.     

Analysis of tea catechins in vegetable oils by high‐performance liquid chromatography combined with liquid–liquid extraction

In this study, a method was developed for the determination of various tea catechins in vegetable oils. Firstly, vegetable oils including tea seed oil, sunflower seed oil and soya bean oil were extracted by methanol/water (40:60, v/v), and then, a high‐performance liquid chromatography (HPLC) method was developed for the simultaneous determination of GA, caffeine, EGC, EGCG, EC, ECG, GC, GCG, C and CG. For the compounds detected in tested vegetable oils, LODs were in the range of 0.05–1.65 ng, both intraday and interday relative standard deviations (RSDs) were <5.0%, and the recovery rates were in the range of 96.2–100.5% with RSD <3.7%. The results showed in vegetable oils which declared to had added tea catechins in, the concentrations of tea catechins were less than that showed in package label, and the content of EGCG was the highest in all samples. Therefore, the advancement made in our study will facilitate studies of tea catechins in oil industry.     

基于同步荧光光谱的杜仲籽油掺假检测研究

建立基于同步荧光光谱的杜仲籽油掺假判别分析模型及检测方法。以杜仲籽油和7种常见植物油为研究对象,采集激发波长范围为250～700 nm,波长间隔为60 nm的同步荧光光谱,分析杜仲籽油和常见食用油的荧光光谱特性,利用光谱峰面积建立掺假判别模型并对其进行验证。结果表明:杜仲籽油与其他7种植物油的荧光特性存在显著差异;分别利用600～700 nm和300～500nm波长范围同步荧光光谱进行主成分分析,其对杜仲籽油掺假识别准确率高达100%;利用峰面积与掺假比例建立定量判别分析模型,检测限分别为1%和0. 48%。该方法可实现对杜仲籽油掺假的定性和定量分析,且具有较高的灵敏度、简便和快速等特点。     

Detection of adulteration in milk: A review

Milk is a wholesome nutritious dairy product and is consumed by a majority of the population worldwide for drinking as such, as well as via dairy products. However, the practice of adulteration of milk invariably reduces its quality and may introduce hazardous substances into the dairy supply chain jeopardising consumers’ health. Various instances of adulteration of milk have been reported globally, wherein substances such as extraneous water, foreign proteins, whey proteins, melamine and urea, vegetable or animal fats, plus many minor constituents of milk fat have been added as potential adulterants in milk and milk products. This review focusses on the different methods of detection of these adulterants in milk using techniques such as DSC, RP‐HPLC, LC‐GC, HPTLC, immunoassays: CE, ELISA, FAMPST, FTIR, NIR spectroscopy, PAGE, IEF, DNA‐based methods and MALDI‐MS that have been developed and employed for the last 25 years. The combination of advanced IR spectroscopy and chemometrics provides a powerful tool for quality and authenticity analysis of milk. An electronic tongue is an easy and economic tool for the detection of caprine milk adulterations with bovine milk. Biosensors having the ability to furnish real‐time signals have been developed for the detection of urea in milk. An attempt has been made to give a clear understanding of the most suitable methods for the determination of various sources of adulteration.     

Authentication of Olive Oil Adulterated with Vegetable Oils Using Fourier Transform Infrared Spectroscopy

Determination of the authenticity of extra virgin olive oils has become more important in recent years following some infamous adulteration and contamination scandals. The study focused on application of Fourier transform infrared spectroscopy to identify the adulteration of olive oils. Single-bounce attenuated total reflectance measurements were made on pure olive oil and olive oil samples adulterated with varying concentrations of sunflower oil (20-100 mL vegetable oil/L of olive oil). Discriminant analysis using 12 principal components was able to classify the samples as pure and adulterated olive oils based on their spectra. A partial least squares model was developed and used to verify the concentrations of the adulterant. Furthermore, the discriminant analysis method was used to classify olive oil samples as distinct from other vegetable oils based on their infrared spectra.     

食用油中掺入低价动物油脂鉴别方法的研究进展

动物油脂是动物脂肪组织经提取精炼而成的油脂。动物油脂因资源丰富,具有独特风味,广泛应用于食用油、起酥油、制备肉味香精,同时也是生产肥皂、甘油和饲料的重要原料。因动物油脂成本低廉,不法商贩受利益驱使在食用植物油或高价动物油脂中掺加低价动物油脂,严重扰乱了市场秩序,侵害消费者合法权益和身体健康。近年来,近红外光谱法与拉曼光谱等光谱法、气相色谱与液相色谱及其质谱联用技术、实时分析质谱、低场核磁共振等技术应用于动物油脂掺假鉴别技术研究。本文对主要动物油脂掺假鉴别技术进行综述,并对其发展趋势进行了综述,以期为动物油脂的掺假鉴别技术研究提供参考。     

电子鼻鉴别核桃油中掺入大豆油、菜籽油及玉米油研究

为了快速简便地鉴别核桃油掺伪,利用电子鼻技术鉴别核桃油中掺入大豆油、菜籽油及玉米油,并采用主成分分析(PCA)和线性判别式分析(LDA)对结果进行分析,研究表明:采用PCA方法可以鉴别核桃油掺入大于20%大豆油、7%菜籽油和7%玉米油;采用LDA方法可以鉴别核桃油中掺入大于1%大豆油、1%菜籽油和7%玉米油,LDA方法比PCA方法能更加有效地鉴别核桃油中掺入大豆油、菜籽油和玉米油的现象。电子鼻技术可以作为鉴别核桃油掺假的一种快速简便的检测技术。     

基于机器学习算法的食用植物油掺伪鉴别的研究进展

市场上存在用低值低价油脂掺伪高值高价食用植物油的现象,这不仅损害食用植物油生产者和消费者利益,也不利于我国食用油脂产业的健康发展。许多学者将机器学习算法应用到食用植物油掺伪鉴别的研究中,取得了显著的研究成果。为了对食用植物油掺伪鉴别的研究和应用提供一定的理论依据和方法参考,总结了国内外现阶段使用机器学习算法进行食用植物油掺伪鉴别的研究进展,这些机器学习算法包括主成分分析、判别分析、支持向量机、随机森林、人工神经网络等。对所述机器学习算法应用于食用植物油掺伪鉴别研究的优缺点进行了分析,在实际应用中应结合实际情况,综合考量选择合适的算法。     

Detection of olive oil adulteration with some plant oils by GLC analysis of sterols using polar column

A new method was developed to determine the presence of some refined vegetable oils in olive oil based on the sum of campesterol and stigmasterol percentages. Model systems of corn, soybean, sunflower and cotton seed oils in olive oil at levels of 5%, 10% and 20% were prepared. The unsaponifiables of these model systems were analysed by GLC using polar column with high thermal stability. An olive oil authenticity factor based on the summation of campesterol and stigmasterol percentages was established as an indicator of olive oil adulteration with vegetable oils. The results indicate the possibility to detect the presence as little as 5% of these plant oils in olive oil.     

Characterization of fatty acid profile by FFFS

The purpose of the study was to assess potential application of front face fluorescence spectroscopy as a rapid and non-destructive technique to discriminate between fats of animal and plant origin based on their fatty acid profiles, and to predict concentration of fatty acids from fluorescence spectra. Vitamin E emission spectra (300–500 nm) of butterfat and vegetable oil samples were recorded with excitation wavelength set at 295 nm. Fatty acid composition of the samples was determined by gas chromatography. Principal component analysis and partial least squares regression analysis were applied to the gas chromatography and fluorescence spectroscopy data. The butter-fats and vegetable oils were discriminated based on the total saturated and unsaturated fatty acids respectively. Tocopherols and tocotrienols accounted for the variability among various oils. A good prediction model was established with R ² = 0.745–0.992 for saturated fatty acids. The unsaturated fatty acids were characterized by low coefficients of determination (R ² < 0.339). The fatty acid profiles predicted from fluorescence spectra did not show significant difference to those determined by gas chromatography used as references. A good association was established between the two data tables. The study demonstrated great potential of front face fluorescence spectroscopy to rapidly discriminate between fats of animal and plant origin, and predict their saturated fatty acids composition, which could in turn be used for detection of milk fat adulteration with vegetable oil.     

基于GC-IMS分析三种植物油炒制海鲈鱼鱼松中挥发性风味物质的研究

本研究以海鲈鱼鱼松为研究对象,通过感官评分、色差和质构确定了植物油最佳添加量为3%。在此基础上,采用气相色谱-离子迁移谱（Gas Chromatography-Ion Mobility Spectroscopy,GC-IMS）技术深入分析了三种植物油（花生油、棕榈油和葵花籽油）炒制鱼松过程中挥发性风味物质的组成情况。结果表明,三种植物油炒制的鱼松中共鉴定出40种挥发性风味物质,包括醛类、醇类、酯类和酮类化合物等,其中,花生油、棕榈油和葵花籽油炒制鱼松中醛类的相对含量最高,分别为63.33%、57.58%和43.75%。不同植物油炒制鱼松中存在特征风味物质,其中,丙醛、苯甲醛分别只存在于花生油、棕榈油炒制鱼松中;3-甲基-1-丁醇和己醛同时存在于花生油和葵花籽油炒制鱼松中。本研究结果表明根据GC-IMS建立的三种植物油炒制鱼松指纹图谱相似度较低,能有效区分炒制鱼松的植物油来源,可作为植物油炒制鱼松的鉴定及掺伪鉴别的有效手段。     

Discriminant Analysis of Selected Edible Fats and Oils and Those in Biscuit Formulation Using FTIR Spectroscopy

Recently, lard adulteration has highlighted the importance of checking raw materials and food products in order to assure their authenticity. Discriminant analysis (DA) using selected frequency regions (3,050?C2,800, 1,800?C1,600, and 1,500?C650 cm^?1) was exploited for the classification of lard and other commercial vegetable oils and animal fats. As a result, the Cooman plot showed that all vegetable fats/oils and animal fats, including lard, are clustered in a distinct group. DA was also employed to assign real food samples, in particular biscuit, into one of two groups. In addition, DA is a very useful means for Halal screening technique in order to enhance the Halal authentication process.     

Influence of composition on degradation during repeated deep‐fat frying of binary and ternary blends of palm,sunflower and soybean oils with health‐optimised saturated‐to‐unsaturated fatty acid ratios

The American Heart Association recommended the fatty acid balance contributed by all the fats in our diet, suggesting it would be best at approximately 1:1:1 for saturated (SFA), monounsaturated (MUFA) and polyunsaturated fatty acids (PUFA), respectively. Three individual oils: palm oil (PO), soybean oil (SBO) and sunflower oil (SNF) and their binary and ternary blends were prepared and used for repeated deep‐fat frying of French fries. The acid value, peroxide value, p‐anisidine value and Totox values, as well as oxidative stability, contents of total polar compounds, tocochromanols, triacylglycerol dimers and oligomers, were determined in individual and blended oils. The lowest Totox value and highest stability were found for PO, and the opposite data were obtained for SNF and SBO. The degradation of tocochromanols in blends ranged from 91% to 95% after 4 days of frying, while in individual oils, it was 63% in SBO, 71% in SNF and 100% in PO. The lowest formation of dimers and oligomers was observed for the PO: SNF blend. Obtained results showed that only pure PO was a better frying medium than its blends with SBO and SNF. However, a prepared blend had a better fatty acid composition for human health and was more stable than pure SBO and SNF.     

基于稳定碳同位素示踪技术的商品植物油掺杂鉴别研究

本文旨在运用所建立的纯植物油的脂肪酸组成及其稳定碳同位素比值判别标志对广州市售商品植物油是否掺杂进行判识。先在广州某大型超市购得18种商品植物油(包括3种茶籽油、5种花生油、2种葵花油、2种玉米油和6种橄榄油);然后采用气相色谱-质谱联用仪(GC-MS)、气相色谱-同位素比值质谱仪(GC-IRMS)和元素分析-同位素比值质谱仪(EA-IRMS)对这18种商品油的脂肪酸组成和全油及其脂肪酸的稳定碳同位素比值进行测定;最后将本次检测所获得的数据与作者之前建立的判别标志进行对比分析。对比结果表明,本批商品植物油的品质总体较好,但其中50%的植物油商品存在掺杂。因此,将植物油脂肪酸组成数据与其稳定碳同位素比值数据相结合,可灵敏地确定待检植物油是否存在掺杂。     

Authentication of edible vegetable oils adulterated with used frying oil by Fourier Transform Infrared Spectroscopy

The application of Fourier Transform Infrared (FTIR) Spectroscopy to authenticate edible vegetable oils (corn, peanut, rapeseed and soybean oil) adulterated with used frying oil was introduced in this paper. The FTIR spectrum of oil was divided into 22 regions which corresponded to the constituents and molecular structures of vegetable oils. Samples of calibration set were classified into four categories for corn and peanut oils and five categories for rapeseed and soybean oils by cluster analysis. Qualitative analysis of validation set was obtained by discriminant analysis. Area ratio between absorption band 19 and 20 and wavenumber shift of band 19 were treated by linear regression for quantitative analysis. For four adulteration types, LODs of area ratio were 6.6%, 7.2%, 5.5%, 3.6% and wavenumber shift were 8.1%, 9.0%, 6.9%, 5.6%, respectively. The proposed methodology is a useful tool to authenticate the edible vegetable oils adulterated with used frying oil.