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1.
Edible oils are used in the preparation of foods as a part of their recipe or for frying. So to ensure of food safety, checking the quality of the oils before and after usage is an important subject in food control laboratories. In this study, edible oils from four different sources (canola, corn, sunflower and frying) were heated for 36 h at 170 °C and sampling was done every 6 h. The free fatty acid, peroxide value and the content of some fatty acids (C16:0, C18:0, C18:1, C18:2, C18:3) of the oil samples were determined by standard methods. Then, the ATR-FTIR spectra of the samples were collected. The partial least squares (PLS) regression combined with genetic algorithm was performed on the spectroscopic data to obtain the appropriate predictive models for the simultaneous estimation of acid value, peroxide value and the percentage of five kinds of fatty acids. The effect of some preprocessing methods on these models was also investigated. Preprocessing of data by orthogonal signal correction (OSC) resulted in the best predictive models for all oil properties. The correlation coefficients of calibration set (>0.99) and validation set (>0.86 and in most case >0.94) of the OSC–PLS model suggested suitable predictive modeling for all studied parameters in the oil samples. This method could be suggested as a rapid, economical and environmental friendly technique for simultaneous determination of seven noted parameters in the edible oils.  相似文献   

2.
The use of near infrared spectroscopy (NIRS) for rapid determination of the degree of interesterification of blends of palm stearin, coconut oil, and rapeseed oil obtained using an immobilized Thermomyces lanuginosa lipase at 70 °C was investigated. Interesterification was carried out by applying both fixed bed and batch reactors. Calibrations were developed for quantitative determination of solid fat content (SFC) at 10, 20, 30, 35, and 40 °C and free fatty acid (FFA) resulting in root mean square errors of prediction of 1.0, 1.3, 1.4, 1.6, 1.7, and 0.19% (w/w), respectively. The data showed that NIRS could be used to replace the traditional methods for determining FFA and SFC in vegetable oils.It was possible to monitor the activity of the immobilized enzyme for interesterification of margarine oils by predicting the equivalent reaction time in a batch reactor from NIR spectra. Root mean square errors of prediction for two different oil blends interesterified for 300 and 170 min were 21 and 12 min, respectively.  相似文献   

3.
Goncalves IM  Murillo M  González AM 《Talanta》1998,47(4):1033-1042
An efficient method was developed for the determination of metals in used lubricating oils, by atomic absorption spectrometry. Oil samples were treated with an acid mixture and then emulsified in water (10% w/w) using ethoxy nonylphenol (6% w/w) as surfactant. Emulsion characteristics (oil, surfactant content and acid mixture) were optimized to obtain the best AAS signal. Good agreement was found between calibration curves of aqueous and emulsified standard solutions when a peristaltic pump was used to introduce the solutions into the flame. The emulsion methodology was comparable, within 95% of confidence, to traditional ashing methodologies when a standard reference oil and a used lubricating oil were analyzed. Precision between 0.4 and 5% RSD was obtained when real sample was analyzed using emulsions.  相似文献   

4.
The behaviour of a single-bore high-pressure pneumatic nebulizer (SBHPPN) as a tool for the analysis of lubricating oils by flame atomic absorption spectrometry (FAAS) was investigated. The effects of the sample oil content [from 10% to 100% (w/w) oil in 4-methylpentan-2-one, IBMK] and the carrier nature (IBMK and methanol) on the characteristics of the aerosols generated, on the analyte transport efficiency and on the analytical figures of merit in FAAS were studied. A pneumatic concentric nebulizer (PCN) was used for comparison. Increasing the oil content increases the viscosity of the sample. With the PCN this gives rise to coarser aerosols, making it impossible to nebulize samples with an oil content higher than 70% (w/w). Using the SBHPPN, the viscosity of the sample scarcely affects the characteristics of the primary aerosols. Hence, the SBHPPN is able, by using the appropriate carrier, to nebulize pure lubricating oils. Among the carriers tested, IBMK is the most advisable because it is fully miscible with all the oil samples. The SBHPPN provides higher sensitivities and lower limits of detection than the PCN. Compared with a method based on organic dilution, the use of the SBHPPN for the direct analysis of lubricating oils by FAAS makes it possible, in addition to increasing the analysis throughput, to detect elements at lower concentrations. Moreover, the SBHPPN provides similar results to those obtained using a previous acid digestion step.  相似文献   

5.
Some vegetable oils such as canola (CaO), corn (CO), soybean (SO), and walnut (WO) oils have similar color with cod liver oil (CLO), therefore, the presence of these oils was difficult to detect using naked eye. For this reason, Fourier transform infrared (FTIR) spectroscopy using horizontal attenuated total reflectance (HATR) as sampling accessory and in the combination with chemometrics was developed for detection and quantification of these vegetable oils as adulterants in CLO. The quantification of vegetable oils was carried out by using multivariate calibrations of partial least squares (PLS) and principle component regression (PCR), while the classification between pure CLO and CLOs adulterated with CaO, CO, SO, and WO was performed using discriminant analysis (DA). PLS with FTIR normal spectra was more suitable compared with PCR for quantification purposes with coefficient of determination (R2) higher than 0.99 and root mean square error of calibration (RMSEC) in the range of 0.04-0.82% (v/v). The PLS model was further used to predict the levels of these vegetable oils in independent samples for validation/prediction purpose. The root mean square error of prediction (RMSEP) values obtained were of 1.75% (v/v) (CaO), 1.39% (v/v) (CO), 1.35% (v/v) (SO), and 1.37% (v/v) (WO), respectively. The classification using DA revealed that the developed method can classify CLO and that mixed with these vegetable oils using 9 principal components.  相似文献   

6.
In this work, multivariable calibration models based on middle- and near-infrared spectroscopy were developed in order to determine the content of biodiesel in diesel fuel blends, considering the presence of raw vegetable oil. Soybean, castor and used frying oils and their corresponding esters were used to prepare the blends with conventional diesel. Results indicated that partial least squares (PLS) models based on MID or NIR infrared spectra were proven suitable as practical analytical methods for predicting biodiesel content in conventional diesel blends in the volume fraction range from 0% to 5%. PLS models were validated by independent prediction set and the RMSEPs were estimated as 0.25 and 0.18 (%, v/v). Linear correlations were observed for predicted vs. observed values plots with correlation coefficient (R) of 0.986 and 0.994 for the MID and NIR models, respectively. Additionally, principal component analysis (PCA) in the MID region 1700 to 1800 cm− 1 was suitable for identifying raw vegetable oil contaminations and illegal blends of petrodiesel containing the raw vegetable oil instead of ester.  相似文献   

7.
利用近红外光谱技术对食用植物油中反式脂肪酸(Trans fatty acids,TFA)含量进行快速定量检测,并通过波段选择、预处理方法、变量筛选及建模方法对TFA含量预测模型进行优化.采用AntarisⅡ傅里叶变换近红外光谱仪在4000~10000 cm-1光谱范围采集98个食用植物油样本的近红外透射光谱,然后采用气相色谱法测定TFA的真实含量.首先,对样本原始光谱进行波段、预处理方法优选;在此基础上,采用竞争自适应重加权法(Competitive adaptive reweighted sampling,CARS)筛选TFA相关的重要变量,最后应用主成分回归、偏最小二乘和最小二乘支持向量机方法分别建立食用植物油中TFA含量的预测模型.研究结果表明,近红外光谱技术检测食用植物油中的TFA含量是可行的,优化后的最佳预测模型的校正集和预测集R2分别为0.992和0.989,RMSEC和RMSEP分别为0.071%和0.075%.最佳预测模型所用的变量仅26个,占全波段变量的0.854%.此外,与全波段偏最小二乘预测模型相比,其预测集R2由0.904上升为0.989,RMSEP由0.230%下降为0.075%.由此表明,模型优化非常必要,CARS能有效筛选TFA相关的重要变量,极大减少建模变量数,从而简化预测模型,并较大提高预测模型的精度和稳定性.  相似文献   

8.
A novel, cost-efficient method for the analytical extraction of the Fusarium mycotoxin zearalenone (ZON) from edible oils by dynamic covalent hydrazine chemistry (DCHC) was developed and validated for its application with high performance liquid chromatography-fluorescence detection (HPLC-FLD). ZON is extracted from the edible oil by hydrazone formation on a polymer resin functionalised with hydrazine groups and subsequently released by hydrolysis. Specifity and precision of this approach are superior to liquid partitioning or gel permeation chromatography (GPC). DCHC also extracts zearalanone (ZAN) but not α-/β-zearalenol or -zearalanol. The hydrodynamic properties of ZON, which were estimated using molecular simulation data, indicate that the compound is unaffected by nanofiltration through the resin pores and thus selectively extracted. The method's levels of detection and quantification are 10 and 30 μg/kg, using 0.2 g of sample. Linearity is given in the range of 10–20,000 μg/kg, the average recovery being 89%. Bias and relative standard deviations do not exceed 7%. In a sample survey of 44 commercial edible oils based on various agricultural commodities (maize, olives, nuts, seeds, etc.) ZON was detected in four maize oil samples, the average content in the positive samples being 99 μg/kg. The HPLC-FLD results were confirmed by HPLC–tandem mass spectrometry and compared to those obtained by a liquid partitioning based sample preparation procedure.  相似文献   

9.
A novel analytical approach has been developed and evaluated for the quantitative analysis of a selected group of widely used pesticides (dimethoate, simazine, atrazine, diuron, terbuthylazine, methyl-parathion, methyl-pirimiphos, endosulfan I, endosulfan II, endosulfan sulphate, cypermethrin and deltamethrin), which can be found at trace levels in olive oil and olives. The proposed methodology is based on matrix solid-phase dispersion (MSPD), (with a preliminary liquid-liquid extraction in olive oil samples) using aminopropyl as sorbent material with a clean-up performed in the elution step with Florisil, followed by mass spectrometric identification and quantitation of the selected pesticides using both gas chromatography-mass spectrometry (GC-MS) in selected ion monitoring (SIM) mode and liquid chromatography tandem mass spectrometry (LC-MS-MS) in positive ionization mode. The recoveries obtained (with mean values between 85 and 115% (obtained at different fortification levels) with RSD values below 10% in most cases, confirm the usefulness of the proposed methodology for the analyses of these kind of complex samples with a high fat content. Moreover, the obtained detection limits, which were below 5 microg kg(-1) by LC-MS analyses and ranged from 10 to 60 microg kg(-1) by GC-MS meet the requirements established by the olive oil pesticide regulatory programs. The method was satisfactorily applied to different olives and olive oil samples.  相似文献   

10.
建立了一种简便、灵敏、无需内标的检测油脂中三酰甘油氧化聚合物(TGP)的分析方法。以制备型快速层析柱(PFC)(flash硅胶柱,20 g,40~60μm,6 nm)分离1 g油脂样品中极性组分(PC),经高效体积排阻色谱(HPSEC)(GPC柱,Ф7.8 mm×300 mm,粒径5μm,孔径10 nm)将PC细分为氧化三酰甘油寡聚物(TGO)、氧化三酰甘油二聚物(TGD)、氧化三酰甘油单体(ox-TGM)、二酰甘油(DG)、游离脂肪酸(FFA)。结合重量法测定油脂中PC、面积归一法测定PC中TGP,可准确定量油脂中的TGP含量。结果表明,TGO、TGD分别在28~1 800、11~2 800 mg/L范围内线性关系良好,相关系数(r2)分别为0.998 2、0.998 7,TGO及TGD的检出限(LOD)分别为28、11 mg/L,定量下限(LOQ)分别为113、44 mg/L;相当于油脂中TGP的LOD为0.01%。PFC-HPSEC法检测油脂TGP的相对标准偏差(RSD)均小于10%。PFC对3个PC加标水平(2.27%、8.47%、30.94%)的平均回收率为95%~98%,相对标准偏差(RSD)均低于4%。PFC-HPSEC方法与经典的硅胶柱-HPSEC方法定量油脂TGP的结果吻合度高,相对误差为0~8.9%。该方法能够在2 h内实现各种油脂中TGP含量的定量检测,包括使用过的废弃油脂与未使用的食用油脂,尤其适用于低含量TGP的初榨油和精炼油脂。  相似文献   

11.
Duong CT  Roper MG 《The Analyst》2012,137(4):840-846
Free fatty acid (FFA) compositions are examined in feedstock for biodiesel production, as source-specific markers in soil, and because of their role in cellular signaling. However, sample preparation of FFAs for gas chromatography-mass spectrometry (GC-MS) analysis can be time and labor intensive. Therefore, to increase sample preparation throughput, a glass microfluidic device was developed to automate derivatization of FFAs to fatty acid methyl esters (FAMEs). FFAs were delivered to one input of the device and methanolic-HCl was delivered to a second input. FAME products were produced as the reagents traversed a 29 μL reaction channel held at 55 °C. A Design of Experiment protocol was used to determine the combination of derivatization time (T(der)) and ratio of methanolic-HCl:FFA (R(der)) that maximized the derivatization efficiencies of tridecanoic acid and stearic acid to their methyl ester forms. The combination of T(der) = 0.8 min and R(der) = 4.9 that produced optimal derivatization conditions for both FFAs within a 5 min total sample preparation time was determined. This combination of T(der) and R(der) was used to derivatize 12 FFAs with a range of derivatization efficiencies from 18% to 93% with efficiencies of 61% for tridecanoic acid and 84% for stearic acid. As compared to a conventional macroscale derivatization of FFA to FAME, the microfluidic device decreased the volume of methanolic-HCl and FFA by 20- and 1300-fold, respectively. The developed microfluidic device can be used for automated preparation of FAMEs to analyze the FFA compositions of volume-limited samples.  相似文献   

12.
Commercial stoned table olives named "alcaparras" from Trás-os-Montes (Portugal) were chemically characterized. During three consecutive years (2004-2006) 30 samples (10 per year) were examined for their nutritional value (moisture, crude protein, total fat, ash, carbohydrates, and energy), with a detailed report of the fatty acids and tocopherols composition. Water was the major constituent (72.5 ± 5.5%), followed by fat (14.6 ± 5.1%). The average amount of protein and ash were 1.1% and 3.4%, respectively, reporting unusual ash values for table olives, related to the technological process. One hundred grams of fresh stoned table olives presented an average energetic value of 156 kcal, lower than most table olives. The lipids are rich in oleic acid (average of 77.7 ± 2.0%), followed by palmitic acid and linoleic acid. Samples showed an average of total tocopherols of 1.2 mg/100 g of fresh weight, being α-tocopherol the most abundant. Table olives are important sources of MUFA, as olive oil, recognized as a preventive factor in diseases in which free radicals are implicated, complemented by the amounts of vitamin E, with both antioxidant and vitamin action.  相似文献   

13.
A high-performance liquid chromatography (HPLC) unit equipped with size exclusion column and a refractive index detector was used for simultaneous monitoring, identification, and quantitation of the reaction components from lipase-catalyzed transesterification of three oils. The procedure simultaneously separated and detected the unreacted triacylglycerols (TAG), diacyl-, and monoacyl-glycerol (DAG and MAG) co-products, residual alcohol as well as free fatty acid (FFA) based on retention times. The chromatograms showed well separated and resolved peaks. The elution of the components from the transesterification reaction in increasing order was: TAG < DAG < FFA < MAG. Generally, higher alcohol ratios decreased the conversion of TAG in all the oils studied with between 14% and 94% of TAG remaining at all the treatment combinations. Higher amount of salmon skin oil (SSO) TAG was generally converted to DAG than Rothsay composite (RC) and olive oil (OO) TAG. Relatively higher amount of OO DAG was converted to MAG than SSO and RC with only 5–14% DAG remaining in OO. RC and OO generally accumulated less MAG, and this was reflected as lower MAG levels in RC (<6%) and OO (<14%) compared with SSO (<27%). For the various treatment combinations and the three oils used in this study, the least amount of FFA was recorded in transesterified OO with a maximum of approximately 4%. This HPLC method can be used as a simple and fast technique to analyze the reaction components and products of transesterification reactions without the need for additional derivatization steps.  相似文献   

14.
A single line flow injection analysis (FIA) method that incorporated a preconcentrator column packed with C(18) particles and capacitively coupled contactless conductivity detector (C(4)D) was developed for the determination of free fatty acid (FFA) in vegetable oils. The carrier stream was methanol/1.5 mM sodium acetate (pH 8) 80:20 (v/v) at a flow rate of 1.0 mL min(-1). Calibration curve was well correlated (r(2)=0.9995) within the range of 1-200 mg L(-1) FFA (expressed as palmitic acid). Sampling rate of 40-60 h(-1) was achieved. Good agreement was found between the standard non-aqueous titrimetry method and the proposed method when applied to the determination of FFA in palm (crude, olein, and refined, bleached and deodorised) and other vegetable (soybean, rice bran, walnut, corn and olive) oils. The proposed method offers distinct advantages over the official method, especially in terms of simplicity, high sampling rate, economy of solvents and sample, offering considerable promise as a low cost automated system that needs minimum human intervention over long periods of time.  相似文献   

15.
Cunninghamella blakesleeana- JSK2, a gamma-linolenic acid (GLA) producing tropical fungal isolate, was utilized as a tool to evaluate the influence of various plant seed oils on biomass, oleagenicity and bio-fuel production. The fungus accumulated 26 % total lipid of their dry biomass (2 g/l) and 13 % of GLA in its total fatty acid. Among the various plant seed oils tested as carbon sources for biotransformation studies, watermelon oil had an effect on biomass and total lipid increasing up to 9.24 g/l and 34 % respectively. Sunflower, pumpkin, and onion oil increased GLA content between 15–18 %. Interestingly, an indigenous biodiesel commodity, Pongamia pinnata oil showed tremendous effect on fatty acid profile in C. blakesleeana- JSK2, when used as a sole source of carbon. There was complete inhibition of GLA from 13 to 0 % and increase in oleic acid content, one of the key components of biodiesel to 70 % (from 20 % in control). Our results suggest the potential application of indigenous plant seed oils, particularly P. pinnata oil, for the production of economically valuable bio-fuel in oleaginous fungi in general, and C. blakesleeana- JSK2, in particular.  相似文献   

16.
In this work, a straightforward, reliable and effective automated method has been developed for the direct determination of monoaromatic volatile BTEXS group (namely benzene, toluene, ethylbenzene, o-, m- and p-xylenes, and styrene) in olives and olive oil, based on headspace technique. Separation, identification and quantitation were carried out by headspace-gas chromatography-mass spectrometry (HS-GC-MS) in selected ion monitoring (SIM) mode. Sample pretreatment or clean-up were not necessary (besides olives milling) because the olives and olive oil samples are put directly into an HS vial, automatically processed by HS and then injected in the GC-MS for chromatographic analysis. The chemical and instrumental variables were optimized using spiked olives and olive oil samples at 50 μg kg−1 of each targeted species. The method was validated to ensure the quality of the results. The precision was satisfactory with relative standard deviations (RSD (%)) in the range 1.6-5.2% and 10.3-14.2% for olive oil and olives, respectively. Limits of detection were in the range 0.1-7.4 and 0.4-4.4 μg kg−1 for olive oil and olives, respectively. Finally, the proposed method was applied to the analysis of real olives and olive oil samples, finding positives of the studied compounds, with overall BTEXS concentration levels in the range 23-332 μg kg−1 and 4.2-87 μg kg−1 for olive oil and olives, respectively.  相似文献   

17.
This paper describes the use of a quick, easy, cheap, effective, rugged, and safe (QuEChERS) method for extraction and cleanup of 16 pesticide residues of interest in olives and olive oil. These products contain a high lipid content, which can adversely affect pesticide recoveries and harm traditional chromatographic systems. For extraction, the main factors (oil and water content) were studied and optimized in experiments to maximize pesticide recoveries. Dispersive SPE with different sorbents was also investigated to minimize matrix coextractives and interferences. For analysis, a new automated DSI device was tested in GC-MS to avoid nonvolatile coextractives from contaminating the instrument. LC-MS/MS with positive ESI was used for those pesticides that were difficult to detect by GC-MS. The final method was validated for olives in terms of recoveries, repeatabilities, and reproducibilities using both detection techniques. The results demonstrated that the method achieved acceptable quantitative recoveries of 70-109% with RSDs < 20% for DSI-GC-MS and 88-130% with RSDs < 10% for LC-MS/MS, and LOQ at or below the regulatory maximum residue limits for the pesticides were achieved.  相似文献   

18.
A substantially more sensitive and accurate alternative to the single-bounce attenuated total reflectance (SB-ATR) Fourier transform infrared spectroscopic method of AOAC/American Oil Chemists' Society (AOCS) was developed for determination of isolated trans isomers, based on transmission measurements using a technique called spectral reconstitution (SR). The method involves the 1:1.5 dilution of an oil with odorless mineral spirits (OMS) containing a spectral marker. The resulting reduction in sample viscosity facilitates the use of a transmission flow cell, with the spectral marker serving to determine the precise dilution ratio. This allows the spectral contributions of the OMS to be eliminated and a facsimile of the neat oil spectrum to be mathematically reconstituted. The transmission-SR (T-SR) procedure was initially evaluated relative to SB-ATR to track changes in the trans content of mixtures of unhydrogenated canola and a highly hydrogenated sunflower oil (0-30% trans). The results indicated that the T-SR procedure had the potential to serve as the basis of an accurate quantitative method. A subsequent T-SR calibration based on the spectral ratioing principle of the SB-ATR AOACIAOCS method was developed by gravimetrically adding trielaidin (0-4%) to extra virgin olive oil (EVO), producing an excellent linear response with a standard deviation (SD) of < 0.04% trans. Subsequent comparison of SB-ATR and T-SR calibrations developed for 5 oils of different types, each spiked with low levels of trielaidin (0-1.2% trans), clearly indicated that SB-ATR was signal-limited, whereas the T-SR procedure performed well. The EVO calibration was subsequently used to predict the added trans content of these spiked oils, after the spectrum of the corresponding unspiked oil had been ratioed out. The resulting plot of predicted versus added trans was linear, with a slope of 1.02 and an overall SD of <0.05% trans. When the spectra of these oils were ratioed against the spectrum of EVO, the trans predictions for some of the oils were offset by 2-3 percentage points, emphasizing the need for the appropriate trans-free reference oil to perform accurate analyses. If the latter condition is met, then T-SR provides a very simple technique, with the potential for automation, for analysis of oils by transmission spectroscopy, with approximately 20x the sensitivity of the AOAC/AOCS SB-ATR method.  相似文献   

19.
This paper proposes an analytical method for simultaneous near-infrared (NIR) spectrometric determination of α-linolenic and linoleic acid in eight types of edible vegetable oils and their blending. For this purpose, a combination of spectral wavelength selection by wavelet transform (WT) and elimination of uninformative variables (UVE) was proposed to obtain simple partial least square (PLS) models based on a small subset of wavelengths. WT was firstly utilized to compress full NIR spectra which contain 1413 redundant variables, and 42 wavelet approximate coefficients were obtained. UVE was then carried out to further select the informative variables. Finally, 27 and 19 wavelet approximate coefficients were selected by UVE for α-linolenic and linoleic acid, respectively. The selected variables were used as inputs of PLS model. Due to original spectra were compressed, and irrelevant variables were eliminated, more parsimonious and efficient model based on WT-UVE was obtained compared with the conventional PLS model with full spectra data. The coefficient of determination (r2) and root mean square error prediction set (RMSEP) for prediction set were 0.9345 and 0.0123 for α-linolenic acid prediction by WT-UVE-PLS model. The r2 and RMSEP were 0.9054, 0.0437 for linoleic acid prediction. The good performance showed a potential application using WT-UVE to select NIR effective variables. WT-UVE can both speed up the calculation and improve the predicted results. The results indicated that it was feasible to fast determine α-linolenic acid and linoleic acid content in edible oils using NIR spectroscopy.  相似文献   

20.
The European food legislation authorizes the use of certain health claims based on a scientific basis. This study aimed to evaluate the fatty acid, tocopherol, and polar phenol composition of virgin olive oil (VOO) from cv. Chondrolia Chalkidikis and Chalkidiki regarding the fulfillment of official requirements for the health claims of ‘oleic acid’, ‘vitamin E’, and ‘olive oil polyphenols’. The examination of representative industrial VOOs from 15 olive mills of the Chalkidiki regional unit showed that the two cultivars yield oils contained the necessary concentrations of the responsible bioactive compounds. This evidence was further substantiated by a four harvest study whereby olives from different maturity stages were sampled from three olive groves. Oils were extracted at a laboratory scale and examined for their content in the above-mentioned three categories of constituents. Oils produced at industrial scale from olives harvested on the ‘technological optimum’ stage according to the olive grove proprietor were also analyzed. Extra virgin olive oil of the studied cultivars can safely bear the generic claims for ‘oleic acid’ and ‘vitamin E’. The cultivars present great potential regarding the total hydroxytyrosol and tyrosol content of the extracted oil required to attain the third health claim that may be influenced negatively by manufacturing practices.  相似文献   

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