A Rapid Method for Simultaneous Analysis of Lignan and γ‐Tocopherol in Sesame Oil by Using Normal‐Phase Liquid Chromatography

A novel method for rapid and simultaneous analysis of three lignans and γ‐tocopherol in sesame oil has been established based on a one‐step solvent extraction followed by normal‐phase liquid chromatography. The briefness of the experimental procedure, use of 5 mL of n‐hexane/isopropanol (98:2, v/v) for extraction without any further cleanup process, short analysis time (10 min), and excellent sensitivity and selectivity demonstrated the advantages of this practical and efficient method. All the analytes exhibited satisfactory recoveries ranging from 95.4 to 103.4% at three spiked levels, with the relative SD ranging from 1.1 to 4.4%. The limits of quantitation of this method for four analytes were in the range of 0.3–1.0 μg g^?1. The validated method was successfully applied to the coinstantaneous determination of lignan and γ‐tocopherol in five real sesame oil samples. Furthermore, the results of this study were compared with previously reported method and standard method.     

Anti-Rancidity Effects of Sesame and Rice Bran Oils on Canola Oil During Deep Frying

In this study, the effect of sesame oil (SEO) and rice bran oil (RBO) on the rancidity of canola oil (CAO) during the process of frying potato pieces at 180 °C was investigated. The SEO and RBO were added to the CAO at levels of 3 and 6%. Frying stability of the oil samples during the frying process was measured on the basis of total polar compounds (TPC) content, conjugated diene value (CDV), acid value (AV), and carbonyl value (CV). In general, frying stability of the CAO significantly (P < 0.05) improved in the presence of the SEO and RBO. The positive effect of the SEO on the stability of the CAO was more than that of the RBO. Increasing the amounts of SEO and RBO from 3 to 6% led to decreases in the TPC and AV, and increases in the CDV and CV of the CAO during the frying process. The best frying performance for the CAO was obtained by use of 3% of both SEO and RBO together (CAO/SEO/RBO, 94:3:3 w/w/w).     

Formation of Benzo(a)pyrene in Sesame Seeds During the Roasting Process for Production of Sesame Seed Oil

The main aim of this research was to enhance the understanding of the formation mechanisms of benzo(a)pyrene (BaP) during roasting of sesame seeds (SS). BaP levels in hot‐ and cold‐pressed sesame seed oil (SSO) were evaluated to correlate oil technology and BaP formation. Extracted principal components from SS were roasted either singly or in mixtures at 230 °C for 30 min. BaP was measured by HPLC with fluorescence detection. The results showed that BaP levels in hot‐pressed SSO were significantly higher than those in cold‐pressed SSO (p < 0.05), BaP formation mostly occurred during SS roasting and increased with roasting temperature (between 80 and 280 °C) and time (from 10 to 50 min). Furthermore, the BaP level in the roasted hulled SS (3.64 μg/kg) was higher than it was in roasted whole SS (1.63 μg/kg). The maximum BaP level observed (5.03 μg/kg) was detected in a roasted mixture of SS protein and SSO. The addition of sesame protein to protein‐free SSO promoted the formation of BaP, which suggests that the pyrolysis products of protein and triacylglycerols are probably important precursors in BaP formation.     

高效微型液相色谱与高温气相色谱联合测定润滑油族组成

采用填充毛细管液相色谱 (PC -HPLC)与高温毛细管气相色谱 (CGC)在线联用技术分析润滑油全组分。PC -HPLC柱 ( 0 .32mmi.d .)用于样品族分离 (烷烃、单环芳烃、双环芳烃、三环芳烃和胶质 )。经PC -HPLC分离后的各族组分被依次存放在多位储存接口内 ,然后分别转入GC作单个族组分的定量分析。该方法是解剖进口润滑油基础油及新产品开发中强有力的分析手段。     

A simplified method for HPLC‐MS analysis of sterols in vegetable oil

We have developed a liquid‐chromatographic method using atmospheric pressure chemical ionization (APCI)‐mass spectrometry (MS) detection in positive mode. This method was used to separate and identify 15 sterols and 2 dihydroxy triterpenes in saponified oils, enabling the analysis of these compounds directly from saponified samples without recourse to thin‐layer chromatography; this fact thus significantly simplifies the process. The analyses were made using a Waters Atlantis 5 µm dC₁₈ 150×2.1 mm column with a gradient of acetonitrile/water (0.01% acetic acid) at a flow rate of 0.5 mL/min and a column temperature of 30 °C. The quantification of several of these compounds in soybean oil, palm oil, seed oil, sunflower oil, olive‐pomace oil and virgin olive oil was carried out using their commercial standards, and the results were compared satisfactorily with the official method.     

Estimating Oil and Protein Content of Sesame Seeds Using Image Processing and Artificial Neural Network

Image processing has many applications in different fields of agriculture. The present study aimed to use image processing techniques and artificial neural networks (ANN) to estimate oil and protein contents of sesame genotypes without the use of time-consuming and costly laboratory methods. The proposed method accurately estimates the parameters in sesame seeds without destructing the genetically valuable material. In this study, a set of 138 morphological features were extracted from the digital image of 125 sesame seed genotypes. A multilayer perceptron (MLP) ANN was then employed to estimate oil and protein contents and determine the relationship between estimated values and laboratory-measured values. The efficiency of this model was compared to radial bases function (RBF), extended RBF (ERBF), GRNN, M5-Rule, M5-Tree, support vector machine regression, and linear regression models. Results showed that MLP performed better in estimating qualitative parameters of seeds in the sesame germplasm. The model estimated oil content with an root mean square error (RMSE) of 2.13% (the accuracy of 97.87%) and an R² of 0.93. Protein content was estimated by an RMSE of 0.378% (the accuracy of 99.62%) and an R² of 0.96.     

Physicochemical Characteristics and Aflatoxin Levels in Two Types of Sudanese Sesame Oil

The physicochemical characteristics and aflatoxin levels of two types of sesame oil [Walad (W) and Normal (N)] were determined. A total of 104 sesame oil samples were collected during two seasons (I and II) from traditional mills in five states of Sudan. Levels of aflatoxin B₁, B₂, G₁, and G₂ were determined using HPLC. The physicochemical characteristics of W and N samples were significantly (P ≤ 0.05) different: samples of W and N from the five states had fluctuations in physicochemical characteristics in the two seasons. The highest percentage of contamination (recorded in Khartoum followed by Kordofan state) by aflatoxin B₁ during season II occurred in normal sesame oil which was 80.77 %, followed by Walad sesame oil which was 76.92 %. These percentages of contamination in season I were lower than 59.26 % for normal sesame oil and lower than 52.0 % for Walad sesame oil in season II. Aflatoxin B₂ contamination recorded the highest incidence in season II (3 out of 26 samples, 11.54 %) of normal sesame oil, followed by Walad sesame oil (2 out of 26 samples, 7.69 %). These percentages were lower than the 7.40 and 4.0 % of normal and Walad sesame oils in season I, respectively. Aflatoxin B₁ and B₂ levels in sesame oil ranged from 0.5 to 9.8 and 0.5 to 1.3 μg/kg, respectively.     

Antioxidant Distributions and Triacylglycerol Molecular Species of Sesame Seeds (Sesamum indicum)

Extracted lipids from sesame (Sesamum indicum) seeds of three varieties were determined by high-performance liquid chromatography (HPLC) for endogenous antioxidants. The molecular species and fatty acid (FA) distribution of triacylglycerol (TAG) isolated from total lipids in sesame seeds were analyzed by a combination of argentation thin-layer chromatography (TLC) and gas chromatography (GC), and were investigated in relation to their antioxidant distribution. γ-Tocopherol was present in highest concentration, and δ-, and α-tocopherols were very small amounts. Sesamin and sesamolin were the main lignan components. A modified argentation-TLC procedure, developed to optimize the separation of the complex mixture of total TAG, provided 12 different groups of TAG, based on both the degree of unsaturation and the total acyl-chain length of FA groups. With a few exceptions, the major TAG components were SM₂ (6.5–6.7%), SMD (19.8–20.7%), M₂D (15.0–26.3%), MD₂ (23.6–35.0%), and D₃ (7.7–10.7%) (where S denotes a saturated FA, M denotes a monoene, D denotes a diene, and T denotes a triene). It seems that the three varieties were highly related to each other based on the FA composition of the TAG as well as the distribution pattern in the different TAG molecular species. These results suggest that there are no essential differences in the oil components among the three varieties.     

Extraction and identification of proanthocyanidins from grape seed (Vitis Vinifera) using supercritical carbon dioxide

In this study, supercritical carbon dioxide extraction of proantocyanidins (PRCs) was performed and the effect of different pressure, temperature and ethanol percentage was investigated. High performance liquid chromatography was used for the analysis of the compounds and it was found that the most effective parameter on the extraction was the amount of the ethanol percentage. Each compound was extracted from grape seeds at their maximum level when different parameters were used which was probably because of their different polarities. Gallic acid (GA), epigallocatechin (EGC) and epigallocatechingallate (EGCG) were extracted at their maximum level when the 300 bar 50 °C and 20% of ethanol was used. The maximum amount of catechin (CT) and epicatechin (ECT) were obtained when 300 bar 30 °C and 20% of ethanol was used for extraction, and 250 bar, 30 °C and 15% of ethanol was needed to extract highest amount of epicatechingallate (ECG).     

Ricinoleic Acid in Common Vegetable Oils and Oil Seeds

An original gas chromatography/mass spectrometry method for quantifying trace amounts of ricinoleic acid (12-hydroxy-cis-9-octadecenoic acid) is detailed. Data are presented on trace amounts of ricinoleic acid found in several common vegetable oils and oils extracted from common oil seeds: e.g., ca. 30 ppm in commercial olive oil was the lowest amount; and ca. 2,690 ppm in oil extracted from cottonseeds was the highest amount.     

Palm oil analysis in adulterated sesame oil using chromatography and FTIR spectroscopy

This study highlights the application of two analytical techniques, namely GC‐FID and FTIR spectroscopy, for analysis of refined‐bleached‐deodorized palm oil (RBD‐PO) in adulterated sesame oil (SeO). Using GC‐FID, the profiles of fatty acids were used for the evaluation of SeO adulteration. The increased concentrations of palmitic and oleic acids together with the decreased levels of stearic, linoleic, and linolenic acids with the increasing contents of RBD‐PO in SeO can be used for monitoring the presence of RBD‐PO in SeO. Meanwhile, FTIR spectroscopy combined with multivariate calibration of partial least square (PLS) has been successfully developed for the detection and quantification of RBD‐PO in SeO using the combined frequencies of 3040–2995, 1660–1654, and 1150–1050 cm^?1. The values of coefficient of determination (R²) for the relationship between actual versus FTIR‐calculated values of RBD‐PO in SeO and root mean square error of calibration (RMSEC) obtained are 0.997 and 1.32% v/v, respectively. In addition, using three factors, the root mean square error of prediction (RMSEP) value obtained using the developed PLS calibration model is relatively low, i.e., 1.83% v/v. Practical Application: The adulteration practice is commonly encountered in fats and oils industry. It involves the replacement of high value edible oils such as sesame oil with the lower ones like palm oil. Gas chromatography and FTIR spectroscopy can be used as reliable and accurate analytical techniques for detection and quantification of palm oil in sesame oil.     

Nondestructive Estimation of Fat Constituents of Sesame (Sesamum indicum L.) Seeds by Near‐Infrared Reflectance Spectroscopy

A rapid and efficient method for oil constituent estimation in intact sesame seeds was developed through near‐infrared reflectance spectroscopy (NIRS) and was used to evaluate a sesame germplasm collection conserved in China. A total of 342 samples were scanned by reflectance NIR in a range of 950–1650 nm, and the reference values for oil content and fatty acid (FA) profiles were measured by Soxhlet and gas chromatograph methods. Useful chemometric models were developed using partial least squares regression with full cross‐validation. The equations had low standard errors of cross‐validation, and high coefficient of determination of cross‐validation (R_c²) values (>0.8) except for stearic acid (0.794). In external validation, r² values of oil and FA composition equations ranged from 0.815 (arachidonic acid) to 0.877 (linoleic acid). The relative predictive determinant (RPD_v) values for all equations were more than 2.0. The whole‐seed NIR spectroscopy equations for oil content and FA profiles can be used for sesame seed quality rapid evaluation. The background information of the 4399 germplasm resources and accessions with high linoleic acid content identified in this study should be useful for developing new sesame cultivars with desirable FA compositions in future breeding programs.     

Sesame Oil and Rice Bran Oil Ameliorates Adjuvant-Induced Arthritis in Rats: Distinguishing the Role of Minor Components and Fatty Acids

Though present in small amounts, the minor constituents of dietary oils may supplement the dietary therapies for rheumatoid arthritis (RA). Hence, in the present study, we assessed the effect of minor constituents from sesame oil (SO) and rice bran oil (RBO) and their fatty acids on the severity of adjuvant‐induced arthritis in experimental rats. Rats were gavaged with 1 mL of SO or RBO or groundnut oil (GNO, control) with or without its minor components for a period 15 days before and 15 days after the induction of arthritis. Oxidative stress, markers of RA, eicosanoids, cytokines, paw swelling and joint integrity were measured in experimental and control rats. Results demonstrated that native SO and RBO but not SO and RBO stripped of their minor components decreased severity of paw inflammation, oxidative stress (lipid peroxides, protein carbonyls, nitric oxide), RA markers (RF and CRP), inflammatory eicosanoids (PGE₂, LTB₄ and LTC₄) and cytokines (IL‐1β, IL‐6, MCP‐1 and TNF‐α) compared to control rats. Native SO and RBO inhibited hydrolytic enzymes (collagenase, elastase and hyaluronidase) in the synovial tissue compared to SO and RBO without minor components. The arthritic scores assessed based on the digital and X‐ray images indicated that native oils but not those without their minor components reduced the paw swelling and bone loss. Our results indicated that minor components of SO and RBO possess a significant degree of an anti‐arthritic effect and are responsible for down regulating inflammation in the experimentally induced arthritis in rats.     

HPLC法测定火麻仁中大麻二酚的含量

本文采用HPLC法对中药火麻仁中大麻二酚进行含量测定。确定色谱条件为：色谱柱Agilent E-clipse XDB-C18（150mm×4.6mm,5μm）;流动相甲醇-水（体积比为78∶22）;流速1.0mL·min^-1;检测波长220nm;柱温25℃。在此条件下,大麻二酚与其它组分得到良好的分离,线性范围为0.04～0.40μg（r=0.9981）,平均加样回收率为95.3%（RSD=0.77%）。     

高效液相色谱法测定含 DIANP 的发射药组分

采用高效液相色谱法测定含１，５－二叠氮基－３－硝基－３－氮杂戊烷的发射药组分。使用烷基柱及乙腈－甲醇－水或甲醇－水混合流动相，可测定ＤＩＡＮＰ、黑索今、硝化甘油、二硝基甲苯和中定剂。     

Extraction of Essential Oils From the Seeds of Pomegranate Using Organic Solvents and Supercritical CO2

In this study, essential oils from pomegranate seeds of the Malas variety from Shahreza, Iran, were extracted using hexane and petroleum benzene applying four extraction methods: normal stirring, soxhlet, microwave irradiation, and ultrasonic irradiation. Also, supercritical fluid extraction (SFE) using CO₂ under different conditions was used for comparison. Different methods of extraction with organic solvents (normal stirring, soxhlet, microwave irradiation, and ultrasonic irradiation) showed significant differences in the extraction yields. However, no differences were found when a given method (e.g., microwave irradiation) was applied using different organic solvents. On the other hand, different extraction conditions from the various runs of SFE resulted in different extraction yields, all of which were lower than those of the other extraction methods using organic solvents. No significant differences were observed in the fatty acid compositions of the extracted oils using organic solvents. However, the fatty acid compositions of the oils extracted under different conditions of the SFE system indicated significant differences among several fatty acids including unsaturated fatty acids.     

Quantitative Determination of Natural Glycolipids from Oil Seed by Automated High‐Performance Thin‐Layer Chromatography (HPTLC)

The role of glycolipids in vegetable oil refining and production of bio‐based fuels has not been disclosed so far. Such investigations required a reliable and reproducible quantitative determination of these compounds. Fundamental data were therefore established on the quantitative determination of glycolipids in vegetable oil gums by means of high‐performance thin‐layer chromatography (HPTLC). Concentrating on five abundant natural glycolipid classes found in these oils, identification of a suitable separation method for the employed glycolipid mixture and those parameters relevant for successful detection were considered in detail. The special importance of sample volume when employing quantitative HPTLC was discussed. Acetone/chloroform/water 6:3:0.4 (v/v/v) was identified as a convenient mobile phase for the investigated issue. A derivatization reagent comprising methanol, copper(II)sulfate pentahydrate, sulfuric acid 98 %, and phosphoric acid 85 % was identified. Subsequent heating at 135 °C for 10 min finished the derivatization and enabled detection at λ = 370 nm. Calibration curves ranging from 1500 to 31.25 ng/mL, regarding both peak area and peak height, were determined. The good correlation of parameters enabled the application of the method to real oil gum samples from sunflower and soybean oil. This revealed that digalactosyldiglycerides in combination with either sterylglucosides or acylated sterylglucosides represented the major glycolipid classes in these oils.     

薄层色谱氢焰离子检测法测定重质油的族组成

建立了快速测定重质油组成的ＴＬＣ／ＦＩＤ法，用３种展开剂可将试样较好地分离为饱和烃、芳烃、胶质和沥青质４个组成。根据大量的实验数据得到了各组分的相对校正因子值，使该方法与经典的液固色谱法有较好的对应关系。该方法精密度高，标准偏差小于３％，比液固色谱法的分析时间大大缩短。     

对甲苯磺酸的高效液相色谱分析

建立了高效液相色谱测定对甲苯磺酸纯度的方法.色谱柱为ODS柱;流动相为水-乙腈-磷酸溶液(体积比为46.7:53.15:0.15),流速0.8 mL/min;紫外检测波长为254 nm;柱温为30 ℃;对甲苯磺酸的质量浓度为22.62～362.00 mg/L时,峰面积与质量浓度具有良好的线性关系,相关系数为0.999 ...     

甲拌膦高效液相色谱检测方法研究

目的探讨高效液相色谱法检测甲拌膦的方法。方法采用不同的流动相、检测波长等反复测定甲拌膦的峰面积与峰高,按照规定的标准方法对本试验条件检测甲拌膦的检测限、线性范围与产品及加标回收率的实验。结果在流动相乙腈+水(85+15)、205 nm波长,甲拌膦在5.1 min附近产生一灵敏色谱峰,线性范围为:0.02~2.5μg,检出限为:0.005μg。结论高效液相色谱在一定条件下测定甲拌膦的含量效果理想。