A simplified method for quantitative analysis of fatty acids in various matrices by gas chromatography is proposed as an alternative to the conventional method and the variables of the protocol examined to optimize the processing conditions. The modified method involves direct methylation of fatty acids in homogenized samples with boron trihalide (BF 3 or BCl 3 in methanol) followed by extraction with hexane. The addition of hexane to the reaction mixture after the methylation process can enhance the efficiency of fatty acid methylation and is critical for those samples that contain high levels of triglycerides. A mechanism underlying this effect is proposed.
Though liquid chromatography electrospray tandem mass spectrometry (LC-ESI-MS(2)) has been widely used in the structural elucidation of triacylglycerols (TAG) in vegetable oils, its potentiality for the identification of TAG molecules in omega-3 rich oils remains unexplored till date. Hence, this article investigates the applicability of LC-ESI-MS(2) for the structural characterization of naturally occurring TAG in cod liver oil without the TAG fractionation during the sample preparation. A computational algorithm was developed to automatically interpret the mass spectra and elucidate the TAG structures respectively. The results were compared against the lipase benchmark method. A principal component analysis study revealed that it is possible to discriminate genuine from adulterated cod liver oil.
Exploring the capabilities of instrumental techniques for discriminating n-3 rich oils derived from animals is a very important though much neglected area that was emphasized more than 100 years ago. In this study the potential of gas chromatography (GC) for discriminating full fatty acid methyl ester (FAME) profiles from fish (cod liver and salmon) and marine mammal (seal and whale) oils is evaluated by means of principal component analysis (PCA). The FAME profiles from plant oils such as rapeseed, linseed and soy oils and seven different brands of n-3 supplements are also used in the discrimination process. The results from the PCA plots can reliably distinguish between plant, n-3 supplements, fish and marine mammal oils. By removing the contribution of the n-3 supplements and plant oils it is possible to discriminate between types of fish and marine animal oils. GC offers a rapid, simple and convenient means of discriminating oils from different species, brands and grades.
The article presents a comprehensive account of the application of chemometric approaches to determine the factors that influence the tri-␣-linolenoylglycerol (TALG) ammoniated adduct signal m/z 890.6 in an ion-trap mass spectrometer coupled to a liquid chromatograph and the estimation of different sources of errors involved in TALG calibration experiments. It was found that by using experimental design, the influence of the nebulizer pressure on the analytical signal is less pronounced than the influence of the drying gas flow and the chromatographic flow rate. The results revealed that without using tandem mass or atmospheric pressure chemical ionization, it is possible to fragment the TALG backbone and obtain the free ␣-linolenic acid by varying the drying gas flow and using an electrospray interface. The error decomposition approach revealed that the preparation error was 26 times higher than the instrumental error. [4,5]. Quantification of TAG using coupled techniques such as LCMS depends mainly on two aspects, the sample preparation technique and the instrumental condition settings. Well-established protocols and books [6 -8] have been devoted to the former and nowadays many research laboratories around the world invest time and resources to investigate new, rapid, and simpler techniques. Works regarding the latter aspect are not widespread in the literature, perhaps because variation of the instrumental conditions can cause drastic alterations to the results obtained with a tested and optimized method [9]. Continuity of results within long periods of time (years) is of paramount importance in clinical studies [10], impairing in some degree the interest in the exploration of new or existing methodologies aiming at optimizing the setting of the LCMS instrumental conditions used in the quantitative analysis of TAG. Superb LCMS instruments equipped with automatic optimization devices could be another reason for the limited number of publications on this field. It has been reported that the sole chromatographic system is influenced by more than 50 factors [11], hence the complexity of chromatography coupled to mass spectrometry overwhelms even the most sophisticated software intended for automatic optimization and method development. The classic one-at-the-time methodology for optimization has been widely used in TAG quantification studies. One of the drawbacks of this method is that it is a tedious procedure and the true optimum can be missed if there are important interactions between the factors. The optimization of a LCMS method is prone to difficulties resulting from the inherent high number of instrumental factors involved and their interactions. The determination of the local response surface and exploitation of the local factor dependence is essential. The discovery and application of methods to that effect are extremely important. This study was undertaken, first to estimate the optimal combination of liquid chromatography-ion-trap-mass spectrometry (LCITMS) experimental variables, specifically nebu...
MgAl layered double hydroxides nanoparticles (LDHs) are known as the useful materials in agrochemsitry. LDHs can be used as a bio-insecticide carrier to enhance insecticide’s activity efficiency. In our study, to improve the insecticide activity of anacardic acid, an extract from cashew nut shell liquid, we intercalated it MgAl layered double hydroxides nanoparticles. Different hybridization between anacardic acid and LDHs (37, 74, 148, and 296µg/mL) (L-As) were made and tested on the survivals of cutworms (Spodoptera litura). L-As or free anacardic acid was sprayed directly on the leaves mustard to feed cutworms or directly on the skin of cutworms. Our results showed that in all L-As treatments, the worm killing efficiency was higher than the free anacardic acid treatment. Hạt nano lớp đôi hydroxides MgAl (LDHs) được biết đến như là những vật liệu hữu ích trong nông ngành hóa học nông nghiệp. LDHs có thể được dùng như là một loại chất mang cho thuốc trừ sâu sinh học để tăng cường hiệu lực diệt sâu. Trong nghiên cứu này, để tăng cường hiệu lực diệt sâu của anacardic acid, một loại hoạt chất được chiết từ dầu vỏ hạt điều, chúng tôi đã gắn chèn nó lên hạt nano lớp đôi hydroxides MgAl. Các nồng độ khác nhau của dạng lai của anacardic và LDHs (37, 74, 148 và 296µg/mL) (L-As) đã được kiểm tra tỷ lệ sống của ấu trùng sâu khoang (Spodoptera litura). Các nghiệm thức L-As và dạng anacardic acid tự do đã được phun lên lá rau cải ngọt cho ấu trùng sâu ăn hoặc phun trực tiếp lên da ấu trùng sâu. Kết quả cho thấy, tất cả các công thức có xử lý bằng L-As, hiệu lực diệt ấu trùng sâu đều cao hơn so với dạng anacardic acid ở trạng thái tự do.
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