基于衰减全反射傅里叶变换红外光谱的餐饮废油掺假检测

为了建立基于衰减全反射傅里叶变换红外光谱(ATR-FTIR)的餐饮废油掺假检测方法,以常见食用油和餐饮废油为原料,收集8个餐饮废油和25个食用油样品,制备30个掺假油样品,共63个油样进行红外光谱扫描。随机取48个油样作为校正集样品,15个油样作为验证集样品,建立餐饮废油定性分析模型,并对定性模型进行验证;从30个掺假油样品中,随机取20个油样作为校正集样品,10个油样作为验证集样品,建立餐饮废油定量分析模型,并对定量模型进行验证。结果表明:在红外光谱范围为1 550~650 cm-1条件下,采用原始光谱结合判别分析建立定性分析模型,其识别率可达100%;采用偏最小二乘法(PLS)建立定量分析模型,在掺假比例1%~10%时,模型预测值与实际掺假比例呈良好的线性关系,相关系数(R)为0.982 2,标准偏差(SD)为0.47。表明基于ATR-FTIR的餐饮废油掺假检测是可行的。     

Chemical characteristics of canarium salomonense oil

Canarium salomonense (ngali nuts) had an oil content of 736 g kg^?1 dry weight. The major fatty acids present were oleic (41–6%), palmitic (34–9%) and stearic (12–6% of the total fatty acids). The nuts produced a yellow oil which had a low free fatty acid content. The fatty acid composition of C salomonense is similar to palm oil and could be used as a general purpose cooking oil.     

GC和LF-NMR结合化学计量学方法检测掺假油茶籽油

为了对油茶籽油品质控制及评价提供支撑,以纯油茶籽油和掺假油茶籽油(分别掺入菜籽油、花生油、棕榈油和高油酸花生油)为试验材料,采用气相色谱法(GC)分析其脂肪酸组成,采用低场核磁共振技术(LF-NMR)测定其横向弛豫特性数据,结合主成分分析(PCA)、偏最小二乘判别分析(PLS-DA)和偏最小二乘分析(PLS)等化学计量学方法建立油茶籽油掺假的定性和定量分析模型。结果表明：5种植物油的脂肪酸组成和LF-NMR横向弛豫特性数据存在显著区别;油茶籽油和其他4种植物油在PCA得分图上可清晰区分;PLS-DA模型可有效区分油茶籽油和掺假油茶籽油,判别正确率均可达100%;建立的油茶籽油中掺入菜籽油、花生油、棕榈油、高油酸花生油的PLS定量预测模型,真实值与预测值的相关系数(R²)分别为0.994 1、0.998 6、0.997 6、0.978 1。综上,GC和LF-NMR结合PCA、PLS-DA以及PLS等化学计量学方法可用于油茶籽油掺假类别判定及掺假量分析。     

三维荧光光谱法快速检测橄榄油中掺假廉价油

目的 建立三维荧光光谱结合机器学习快速检测橄榄油中掺假廉价油的方法。方法 采集橄榄油及掺入大豆油、玉米油、棕榈油三种不同浓度梯度油的荧光光谱数据,利用标准差标准化（standardscaler）、标准正态变换（standard normal variate,SNV）、归一化（normalize）三种光谱预处理方法,基于K近邻(K-nearest neighbor,KNN)、随机森林(random forest,RF)、支持向量机(support vector machine,SVM)、偏最小二乘法(partial least squares,PLS)和卷积神经网络(convolutional neural network,CNN) 5种机器学习方法,构建5种橄榄油定量掺假模型。结果 在定性模型中,基于PLS算法构建的模型效果最好,对3种掺假橄榄油的准确率为79%~97%,其中,在鉴定掺假大豆油的橄榄油中正确率高达97%。在构建的掺假油定量模型中,Standardscaler预处理结合RF算法,构建的定量模型最优,Rc2、Rp2、RMSEC、RMSEP最高,分别为1.00、0.99、0.01、0.02。结论 构建橄榄油掺假3种油的定性定量模型,并建立一种快速、实时、低成本的橄榄油掺假检测方法,能够准确判断是否掺入廉价油,并量化掺假程度,提供更全面的橄榄油质量评估。     

基于傅里叶变换红外光谱的大豆原油掺伪定量 分析模型研究

目的应用傅里叶变换红外光谱(FTIR)结合最小偏二乘法(PLS)建立大豆原油-棕榈油二元掺伪体系的定量分析模型。方法以42个大豆原油、21个精炼油、88个掺伪油的FIIR谱图为模型样本,预处理方法选用标准正态变量(SNV),在此基础上应用主成分分析(PCA)提取特征变量,随机选取60个掺伪油样组成校正集,28个掺伪油样组成验证集,以PLS方法建立大豆原油的掺伪定量模型。结果 PCA可将大豆原油及精炼油分成独立的2类。经PCA分析,大豆原油中掺入棕榈油的掺伪检测限为5%。PLS校正模型的判定系数R2为0.9926,校正误差均方根RMSEC为1.8121。预测模型的R2为0.9823,交叉验证误差均方根RMSECV为2.8189。同时得到的预测结果的偏差在1.3909%~3.1019%之间,差异不显著,说明此模型可行。结论 FTIR-PLS模型能够实现大豆原油的掺伪定量分析,分析速度快,能够满足大豆原油入库要求,是一种可行的大豆原油掺伪分析方法。     

Characterization and authentication of a novel vegetable source of omega-3 fatty acids,sacha inchi (Plukenetia volubilis L.) oil

Consumption of omega-3 fatty acids (ω-3’s), whether from fish oils, flax or supplements, can protect against cardiovascular disease. Finding plant-based sources of the essential ω-3’s could provide a sustainable, renewable and inexpensive source of ω-3’s, compared to fish oils. Our objective was to develop a rapid test to characterize and detect adulteration in sacha inchi oils, a Peruvian seed containing higher levels of ω-3’s in comparison to other oleaginous seeds. A temperature-controlled ZnSe ATR mid-infrared benchtop and diamond ATR mid-infrared portable handheld spectrometers were used to characterize sacha inchi oil and evaluate its oxidative stability compared to commercial oils. A soft independent model of class analogy (SIMCA) and partial least squares regression (PLSR) analyzed the spectral data. Fatty acid profiles showed that sacha inchi oil (44% linolenic acid) had levels of PUFA similar to those of flax oils. PLSR showed good correlation coefficients (R² > 0.9) between reference tests and spectra from infrared devices, allowing for rapid determination of fatty acid composition and prediction of oxidative stability. Oils formed distinct clusters, allowing the evaluation of commercial sacha inchi oils from Peruvian markets and showed some prevalence of adulteration. Determining oil adulteration and quality parameters, by using the ATR-MIR portable handheld spectrometer, allowed for portability and ease-of-use, making it a great alternative to traditional testing methods.     

Detection of adulteration of extra-virgin olive oil by chemometric analysis of mid-infrared spectral data

This study focuses on the detection and quantification of extra-virgin olive oil adulteration with different edible oils using mid-infrared (IR) spectroscopy with chemometrics. Mid-IR spectra were manipulated with wavelet compression previous to principal component analysis (PCA). Detection limit of adulteration was determined as 5% for corn–sunflower binary mixture, cottonseed and rapeseed oils. For quantification of adulteration, mid-IR spectral data were manipulated with orthogonal signal correction (OSC) and wavelet compression before partial least square (PLS) analysis. The results revealed that models predict the adulterants, corn–sunflower binary mixture, cottonseed and rapeseed oils, in olive oil with error limits of 1.04, 1.4 and 1.32, respectively. Furthermore, the data were analysed with a general PCA model and PLS discriminant analysis (PLS-DA) to observe the efficiency of the model to detect adulteration regardless of the type of adulterant oil. In this case, detection limit for adulteration is determined as 10%.     

基于可见—近红外光谱的花生油二元掺伪体系鉴别研究

为了建立一种简便有效的花生油掺伪的定性和定量鉴别方法,采集花生油中分别掺伪0~90%大豆油、棕榈油和棉籽油样品的可见—近红外光谱图,结合主成分分析、判别分析、改进偏最小二乘法,建立花生油掺伪的定性鉴别和定量预测模型。结果表明,在定性鉴别中,对花生油中分别掺入大豆油、棕榈油和棉籽油的整体正确判别率分别达到了100%、96.1%和85.3%。在定量分析中,对MPLS法建立的花生油二元掺伪定标模型进行验证,结果表明,掺入大豆油、棉籽油和棕榈油的预测相关系数R_p~2分别为0.998、0.997和0.995,相对标准差RSD分别为2.33%、3.04%和3.83%,相对分析误差RPD分别为3.542、2.642和2.581,说明这三种掺假花生油所建立的最优定标模型的预测精度高,其中花生油中掺入大豆油的预测精度最高,检测花生油中掺入棉籽油与棕榈油的最低掺假量为3%。为花生油二元掺伪模式提供了一种简便、快速、有效的分析方法。     

Effects of cooking and reheating methods on the fatty acid profile of sea bream treated with rosemary extract

BACKGROUND: The effects of rosemary extract on the fatty acid profile of sea bream fillets cooked by different methods (oven baking, grilling and pan frying) as well as the effects of different reheating methods (microwave and conventional oven) on the fatty acid composition of fish after frozen storage for 4 months were investigated. RESULTS: The proportion of saturated fatty acids increased only slightly in fried samples but significantly in oven‐baked and grilled samples, while the proportion of polyunsaturated fatty acids (PUFAs) increased significantly in fried samples but only slightly in oven‐baked and grilled samples. The proportion of monounsaturated fatty acids remained relatively constant after cooking. Of the fatty acids analysed, the most significant increases (P < 0.05) were observed in C18:1n‐9 and C18:2n‐6 and the most significant decreases (P < 0.05) in C14:0, C16:1, C20:5n‐3 and C22:6n‐3. Although sea bream fillets fried in sunflower oil showed an increase in PUFAs, the lowest eicosapentaenoic and docosahexaenoic acid contents were found in fried samples. CONCLUSION: Sea bream fillets treated with rosemary extract showed slower oxidation than untreated fish. Neither conventional nor microwave reheating after frozen storage for 4 months had a detrimental effect on the fatty acid profile and its stability. Copyright © 2009 Society of Chemical Industry     

Discrimination of olive oil adulterated with vegetable oils using dielectric spectroscopy

The study focused on application of dielectric spectroscopy to identify the adulteration of olive oil. The dielectric properties of binary mixture of oils were investigated in the frequency range of 101 Hz–1 MHz. A partial least squares (PLS) model was developed and used to verify the concentrations of the adulterant. Furthermore, the principal component analysis (PCA) was used to classify olive oil sample as distinct from other adulterants based on their dielectric spectra. The results showed that the dielectric spectra of binary mixture of olive oil spiked with other oils increased with increasing concentration of soy, corn, canola, sesame, and perilla oils from 0% to 100% (w/w) over the measured frequency range. PLS calibration model showed a good prediction capability for the concentrations of the adulterant. For olive oil adulterated with soy oil, the results showed that the RMS was 0.053, sd(RMS), 0.017 and Q² value was 0.967. PCA classification plots for all oil samples showed clear performance in the differentiation for the different concentrations of the adulterant. Each of the oil samples could be easily grouped in different clusters using dielectric spectra. From the results obtained in this research, dielectric spectroscopy could be used to discriminate the olive oil adulterated with the different types of the oils at levels of adulteration below 5%.     

Production of trans‐free margarine stock by enzymatic interesterification of rice bran oil,palm stearin and coconut oil

BACKGROUND: Trans‐free interesterified fat was produced for possible usage as a spreadable margarine stock. Rice bran oil, palm stearin and coconut oil were used as substrates for lipase‐catalyzed reaction. RESULTS: After interesterification, 137–150 g kg^?1 medium‐chain fatty acid was incorporated into the triacylglycerol (TAG) of the interesterified fats. Solid fat contents at 25 °C were 15.5–34.2%, and slip melting point ranged from 27.5 to 34.3 °C. POP and PPP (β‐tending TAG) in palm stearin decreased after interesterification. X‐ray diffraction analysis demonstrated that the interesterified fats contained mostly β′ polymorphic forms, which is a desirable property for margarines. CONCLUSIONS: The interesterified fats showed desirable physical properties and suitable crystal form (β′ polymorph) for possible use as a spreadable margarine stock. Therefore, our result suggested that the interesterified fat without trans fatty acid could be used as an alternative to partially hydrogenated fat. Copyright © 2010 Society of Chemical Industry     

Extra-Virgin Olive Oil and Cheap Vegetable Oils: Distinction and Detection of Adulteration as Determined by GC and Chemometrics

Refined oils including corn, sunflower, soybean, and palm oils as well as low-quality olive oil such as refined lampante and pomace olive oils are commonly used for extra-virgin olive oil (EVOO) adulteration. Indeed, K ₂₇₀ could be used as a parameter for the detection of EVOO fraud for each type of the studied refined oils, 10 % olive, 4 % pomace olive, 10 % palm, 5 % corn, and 2 % soybean oils. Moreover, the adulteration could also be detected by the increase of the trans fatty acid contents with 10 % pomace olive, 3 % soybean, 3 % sunflower, 2 % corn, and 10 % palm oils. Actually, stigmasta-3,5-diene content is one of the most effective means of detecting refined oils in EVOO at low levels: 2 % olive, 0.4 % pomace olive, 1 % palm, 0.2 % soybean, 0.5 % sunflower, and 0.1 % corn oils. Finally, the application of linear discriminant analysis could represent an alternative and innovative tool for faster and cheaper evaluation of EVOO adulteration.     

Use of ATR-FTIR spectroscopy coupled with chemometrics for the authentication of avocado oil in ternary mixtures with sunflower and soybean oils

Avocado oil is a high-value and nutraceutical oil whose authentication is very important since the addition of low-cost oils could lower its beneficial properties. Mid-FTIR spectroscopy combined with chemometrics was used to detect and quantify adulteration of avocado oil with sunflower and soybean oils in a ternary mixture. Thirty-seven laboratory-prepared adulterated samples and 20 pure avocado oil samples were evaluated. The adulterated oil amount ranged from 2% to 50% (w/w) in avocado oil. A soft independent modelling class analogy (SIMCA) model was developed to discriminate between pure and adulterated samples. The model showed recognition and rejection rate of 100% and proper classification in external validation. A partial least square (PLS) algorithm was used to estimate the percentage of adulteration. The PLS model showed values of R² > 0.9961, standard errors of calibration (SEC) in the range of 0.3963–0.7881, standard errors of prediction (SEP estimated) between 0.6483 and 0.9707, and good prediction performances in external validation. The results showed that mid-FTIR spectroscopy could be an accurate and reliable technique for qualitative and quantitative analysis of avocado oil in ternary mixtures.     

Authentication analysis of cod liver oil from beef fat using fatty acid composition and FTIR spectra

This study aimed to authenticate cod liver oil (CLO) from beef fat (BF) by determining the level of BF as a fat adulterant in CLO. Two instrumental techniques, namely GC-FID for fatty acid analysis and Fourier transform infrared (FTIR) spectroscopy, were exploited for such authentication. The decreased level of some fatty acids, especially eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA), could be used as an indicative means to detect the adulteration of CLO with BF. In addition, FTIR spectroscopy combined with partial least-squares (PLS) at frequency regions of 1200–1000?cm^?1 was successfully developed for the quantification of BF in CLO. Using the PLS model, the errors obtained in calibration and prediction samples were 0.55% and 0.82% v/v, respectively.     

Fast simultaneous determination of capsaicin,dihydrocapsaicin and nonivamide for detecting adulteration in edible and crude vegetable oils by UPLC-MS/MS

Capsaicinoids are pungent components in hot peppers, which have been detected in waste cooking oil. However, trace analysis of capsaicinoids in edible and crude vegetable oils is a challenging task due to the complex matrix. In this study, a simple liquid-liquid extraction and solid phase extraction (SPE) coupled with RP-UPLC-ESI-MS/MS method was developed for the quantification of capsaicinoids in edible and crude vegetable oils to screen the adulteration with waste cooking oil. This method was used to simultaneously determine 3 capsaicinoids (capsaicin, dihydrocapsaicin, and nordihydrocapsaicin) with capsaicin-d₃, and dihydrocapsaicin-d₃ as internal standards. This method allows the complete analysis of a sample in only an hour, even including sample preparation and chromatographic separation. The linear range of 3 capsaicinoids ranged between 0.5 and 40 µg/kg. The limit of detection (LOD) and limit of quantification (LOQ) for capsaicinoids were calculated as 0.15 and 0.5 µg/kg, respectively. Quantitative recoveries ranging from 92.9% to 105% were obtained by the analysis of spiked oil. The relative standard deviations were less than 5% (n = 6). The established method can potentially overcome the interference of triacylglycerols and fatty acids in edible and crude vegetable oils, and have been successfully applied to analyse real oil samples. This method provided a rapid and reliable method for the detection of adulteration of vegetable oils with waste cooking oils.     

近红外光谱结合偏最小二乘法用于纯茶油中掺杂菜籽油和大豆油的定量分析

采用偏最小二乘法(PLS)建立了油茶籽油中掺杂菜籽油和大豆油的近红外光谱定量检测模型。配制不同比例(0～100%)的油茶籽油和菜籽油、油茶籽油和大豆油混合样品共256个,采集样品在10000～4000cm-1范围内的近红外透反射光谱,模型采用交互验证和外部检验来考察所建立模型的可靠性,不需进行任何光谱预处理,所建立的PLS模型相关系数为0.9997,训练集的交叉验证均方根误差(RMSECV)为0.504,预测集的预测均方根误差(RMSEP)为0.66。应用建立的模型对未知样品进行预测,并对预测值和真实值进行比较,在掺杂油含量为2.5%～100%之间范围内准确可靠,研究结果表明,采用近红外光谱技术可以实现纯茶油中菜籽油和大豆油掺杂量检测。     

Method development and survey of Sudan I–IV in palm oil and chilli spices in the Washington,DC, area

Sudan I, II, III and IV dyes are banned for use as food colorants in the United States and European Union because they are toxic and carcinogenic. These dyes have been illegally used as food additives in products such as chilli spices and palm oil to enhance their red colour. From 2003 to 2005, the European Union made a series of decisions requiring chilli spices and palm oil imported to the European Union to contain analytical reports declaring them free of Sudan I–IV. In order for the USFDA to investigate the adulteration of palm oil and chilli spices with unapproved colour additives in the United States, a method was developed for the extraction and analysis of Sudan dyes in palm oil, and previous methods were validated for Sudan dyes in chilli spices. Both LC-DAD and LC-MS/MS methods were examined for their limitations and effectiveness in identifying adulterated samples. Method validation was performed for both chilli spices and palm oil by spiking samples known to be free of Sudan dyes at concentrations close to the limit of detection. Reproducibility, matrix effects, and selectivity of the method were also investigated. Additionally, for the first time a survey of palm oil and chilli spices was performed in the United States, specifically in the Washington, DC, area. Illegal dyes, primarily Sudan IV, were detected in palm oil at concentrations from 150 to 24 000 ng ml^–1. Low concentrations (< 21 µg kg^–1) of Sudan dyes were found in 11 out of 57 spices and are most likely a result of cross-contamination during preparation and storage and not intentional adulteration.     

Fatty acid composition and carcass characteristics of growing lambs fed diets containing palm oil supplements

Thirty 45-day-old male Ojalada lambs were used to investigate the effect of palm oil (as such or in the form of calcium soap) on carcass characteristics and fat composition. Dietary palm oil did not significantly affect dorsal fat thickness, carcass fatness or carcass conformation. The palm oil supplement did not affect C16:0 levels in intramuscular and subcutaneous fat, but did increase the percentage of C16:0 and reduce PUFA and MUFA content in internal fat depots. Supplementation with palm oil in the form of calcium soap did not cause significant differences in the composition of intramuscular fat. Subcutaneous and perirenal fat of lambs fed treatments including palm oil as such contained higher levels of some saturated fatty acids than that of those fed fat in the form of calcium soap. Mesenteric fat of lambs that received calcium soap had less % C18:1 and more % C18:3 than that of those given palm oil.     

A study on monitoring of frying performance and oxidative stability of cottonseed and palm oil blends in comparison with original oils

Blending polyunsaturated oils with highly saturated or monounsaturated oils has been studied extensively; however, in literature there is negligible information available on the blending of refined cottonseed oil with palm olein oil. Blending could enhance the stability and quality of cottonseed oil during the frying process. In the present study, the effects of frying conditions on physicochemical properties of the palm olein-cottonseed oil blends (1:0, 3:2, 1:1, 2:3, and 0:1, w/w) were determined and compared to the pure oils. The frying process of frozen French fries was performed in duplicate at 170 ± 5°C for 10 h without interruption. The oil degradations were characterized during deep-frying applications; peroxide, free fatty acid, and iodine value by standardized methods, fatty acid profile by using a gas chromatography-flame ionization detector, polar and polymeric compounds by using the high-performance size exclusion chromatography/evaporative light scattering detector technique. The present study clearly indicated that the oxidative and frying performances of pure palm olein oil and cottonseed oil significantly improved by blending application. Results clearly indicated that the frying performance of cottonseed oil significantly improved by the blending with palm olein oil. Except that free fatty acid content, all the physicochemical variables were significantly influenced by type of pure and blend oils. By increasing the proportion of palm olein oil in cottonseed oil, the levels of polyunsaturated fatty acids decreased, while saturated fatty acid content increased. The progression of oxidation was basically followed by detecting polar and polymeric compounds. The fastest increments for polar and polymeric compounds were found as 6.30% level in pure cottonseed oil and as 7.07% level in 40% cottonseed oil:60% palm olein oil blend. The least increments were detected as 5.40% level in 40% cottonseed oil:60% palm olein oil blend and 2.27% level in 50% cottonseed oil:50% palm olein oil blend. These levels were considerably below the acceptable levels recommended by the official codex. Therefore, the present study suggested that blending of cottonseed oil with palm olein oil provided the oil blends (50% cottonseed oil:50% palm olein oil and 40% cottonseed oil:60% palm olein oil, w/w) with more desirable properties for human nutrition.     

Fatty acid composition and sensory traits of beef fed palm oil supplements

This study measured the effect of replacing dietary fat from an animal source with palm oil supplements on the intramuscular fatty acid profile and sensory quality traits of the meat from young bulls. Thirty-six entire male Friesian calves (mean age=6.8±1.1 months, mean live weight=162.5±28.6kg) were assigned to one of four isoenergetic (1.03 MFU/kg DM) and isoproteinic (15.5% CP) diets, that differed in their fat additives: (D1) lard-tallow mix (control); (D2) hydrogenated palm oil fatty acids (PFA); (D3) calcium salt of partially hydrogenated PFA, and (D4) calcium salt of the fatty acid distillate from palm oil. Bulls (mean live weight=391.3±30.3kg) were slaughtered under commercial conditions and sensory tests were performed to evaluate the effects of the four diets and ageing time (1, 10, and 21d). Only the proportions of C16:0 and C18:0 were significantly affected by the palm oil dietary supplement. Ageing time affected grass odour, tenderness, juiciness, fibrosity, liver flavour, and acid flavour. Nevertheless, palm oil supplements did not negatively alter the organoleptic characteristics of the meat.