Analysis of Cod-Liver Oil Adulteration Using Fourier Transform Infrared (FTIR) Spectroscopy

Analysis of the adulteration of cod-liver oil with much cheaper oil-like animal fats has become attractive in recent years. This study highlights an application of Fourier transform infrared (FTIR) spectroscopy as a nondestructive and fast technique for the determination of adulterants in cod-liver oil. Attenuated total reflectance measurements were made on pure cod-liver oil and cod-liver oil adulterated with different concentrations of lard (0.5–50% v/v in cod-liver oil). A chemometrics partial least squares (PLS) calibration model was developed for quantitative measurement of the adulterant. Discriminant analysis method was used to classify cod-liver oil samples from common animal fats (beef, chicken, mutton, and lard) based on their infrared spectra. Discriminant analysis carried out using seven principal components was able to classify the samples as pure or adulterated cod-liver oil based on their FTIR spectra at the selected fingerprint regions (1,500–1,030 cm⁻¹).     

Compositional and thermal characterization of genuine and randomized lard: A comparative study

Composition and thermal characterization of genuine and randomized lard were investigated comparatively in an attempt to find common merits that assess lard detection. The investigation included compositional and positional distribution of fatty acids, triacylglycerol profiling by gas chromatography (GC) and reversed-phase high-performance liquid chromatography (RP-HPLC), as well as thermal behavior by differential scanning calorimetry (DSC) of both samples. Individual and total saturated and unsaturated fatty acid composition in total fats of both genuine and randomized lard were identical. On the other hand, the results of pancreatic lipolysis/GC analysis showed that the average percent palmitic acid [PAEF(%)] and myristic acid [MAEF(%)] enrichment factors of genuine (280 and 270) and randomized lard (110 and 98) were quite different. Thus, application of PAEF to detect randomized lard is of no value. However, normalization of fatty acid distribution by randomization in 2-monoacylglycerols made the individual and total saturated and unsaturated fatty acids almost identical to that of total fat and neutral triacylglycerols (TG) of lard. TG compositional analysis by GC revealed that both genuine and randomized lard had six dominant TG (C_46′C_48′C_50′C_52′C_54′ and C₅₆) with quite different concentrations. TG with C₅₂ represent the major constituent of genuine and randomized lard. TG profiling of samples was also carried out by RP-HPLC with a refractive index detector. The same peaks were eluted in both samples, but the area % of major peaks changed due to randomization. 2-Palmitooleostearin (SPO) was found in high proportion in lard. However, the ratios of SPO to 2-palmitooleolinolein of both genuine and randomized lard are close (0.6±0.05) and significantly distinguishable from that of beef (4.24), mutton (6.17), chicken (0.21), and turkey (0.14) fats. The DSC thermogram and thermodynamics of phase transitions of both samples were quite different and do not reveal common characteristic(s) that could be used for immediate detection of lard substances in fat admixtures.     

Characteristics of bread and buns made with lard and vegetable oils of different iodine values

A good-quality white loaf of bread or rolls can be baked by substituting liquid vegetable oil (canola, soya and palm) for the standard shortening,i.e. lard, tallow or partially hydrogenated vegetable shortening. Canola oil and soya oil produced lower specific volumes of 5.56 and 5.55 cm³/g and higher softness indices when used with mono- and diglycerides only. Palm oil and lard produced specific volumes of 6.33 and 6.15 cm³/g and lower softness indices with mono- and diglycerides. When a blend of surfactants consisting of mono- and diglycerides and sodium stearyl lactylate (SSL) was used at 0.5% of flour weight, palm, canola, lard and soya gave comparable results in specific volume and compressibility. Rolls baked with the same fats and oils, and addition of ethoxylated stearic acid (MYRJ 45H) or a blend of MYRJ 45H and SSL, all gave good specific volumes ranging from 6.92 to 7.27 cm³/g and a softness index range of 0.71–0.86 and 0.68–0.86 after 48 and 96 h of storage. When a proper surfactant is used, good-quality bread and rolls can be baked with liquid vegetable oil. Furthermore, the usage level of liquid oil can be cut by approximately 30% in comparison to lard or shortening while still maintaining quality.     

Substitutability of fractionated beef tallow for other fats and oils in the food and confectionery industries: An economic evaluation

The United States is the most important beef tallow producer in the world, supplying ca. 5.5 billion pounds annually. Approximately half of this beef tallow is exported at relatively low prices when compared to other fats and oils. Only ca. 10% of the total is used in domestic edible products. On the other hand, cocoa butter, coconut oil, palm oil, and palmkernel oil are imported oils whose demand for use in food and confectionery products has been increasing over the past few years. The first of these is the most expensive fat in the world. Beef tallow contains specific triglycerides which are also contained in these imported fats and oils. Through modern technology, beef tallow has been fractionated into products which are compatible with or superior to the imported fats and oils. It is visualized that products from fractionated beef tallow can be used as substitutes and extenders to cocoa butter, palm oil, and other fats and oils in the food and confectionery industries. The economic evaluation in this paper, analyzed through time series data and multiple regression techniques, established the past relationships between per capita consumption of confectionery food fat, beef tallow, cocoa butter, adjusted per capita disposable income, and adjusted costs of confectionery, beef tallow, and cocoa butter from 1956 to 1973. The substitutability of fats and oils was evaluated and the potential uses of fractionated beef tallow investigated. Presented in part at the AOCS meeting in Cincinnati, September 1975.     

Untersuchungen über die Fettverwertung der Regenbogenforelle (Salmo gairdnerii,R.) III: Einsatz von Leinöl,Maiskeimöl,Olivenöl,Schweineschmalz und Rindertalg im Vergleich zu Sonnenblumenöl in einer gereinigten Futtermischung

Investigations of Fat Utilization of the Rainbow Trout (Salmo gairdnerii, R.) III: Use of Linseed Oil, Maize Germ Oil, Olive Oil, Lard and Tallow in Comparison to Sunflower Oil in a Purified Food Mixture The use of various feeding fats of animal and vegetable origin is reported with respect to the suitability in the nutrition of rainbow trouts. All investigated fat components led to food utilization numbers of <1.0 and PER-values of >2.0. There were no pathological-anatomical modifications of the internal and external organs within the testperiod of ten weeks. Linseed oil led to a better utilization than sunflower oil and lard. The utilization of maize germ oil, olive oil and tallow was only insignificantly lower. All up to now investigated fats seem to be suitable as single components in the only food for rainbow trouts.     

Fractionation of lard and tallow by systematic crystallization

Summary Lard and edible tallow were subjected to a series of fractional crystallizations from acetone at temperatures from 20° to -45°C. Six recrystallized precipitate fractions and a filtrate residue were obtained from each fat. In addition to determining the more common physical and chemical characteristics, fatty acid composition of each fraction was calculated from spectrophotometric data, iodine value, and thiocyanogen value. The consistent results obtained throughout by the spectrophotometric method of fatty acid analysis lend further confirmation to the reliability of this method for composition studies of natural fats. The approximate amounts of tri-saturated, di-saturated, mono-saturated, and tri-unsaturated glycerides of the lard and tallow were estimated from the analysis of each fraction on the assumption that not more than two of these classes of glycerides were present in any one fraction. The tallow contains much higher proportions of tri-saturated and di-saturated glycerides and correspondingly lower proportions of the mono-saturated and tri-unsaturated glycerides than does lard. The amount of tri-unsaturated glycerides in lard was found to be significantly greater than meager information in the literature would indicate. The data indicate that the general pattern of glyceride formation in animals such as the pig and cow is probably of random character. One of the laboratories of the Bureau of Agricultural and Industrial Chemistry, Agricultural Research Administration, U. S. Department of Agriculture. Presented at the 19th fall meeting of the American Oil Chemists’ Society, Chicago, Ill., Nov. 7–9, 1945.     

Turbidimetry for crystalline fractionation of lard

Development of specific properties of lard, a well-known edible animal by-product and one which plays an important role in Chinese-style foods, was studied by means of multiple-step crystalline fractionation. A method for monitoring the crystallization temperature and crystallization time of lard by spectral turbidity was also studied. The capabilities of the proposed method were experimentally demonstrated through recovery of the fat crystal mass. Six significant changes in turbidity spectra, which correspond to the formation of fat crystals, were observed at various temperatures while cooling the melted lard from 50°C to the final vessel temperature at a constant cooling (0.5°C/min) and agitator rate (50 rpm). Crystallization time for each lard fraction was determined while the peak in turbidity was observed in the process of cooling at a specific temperature. Determination of crystallization time by means of turbidimetry correlated with the increase in deposition of fat crystals. No significant increase in fat crystal mass was observed when cooling prolongation after the turbidity peak for the sample was measured. Attributes of lard fractions were characterized by iodine value, saponification value, fatty acid composition, and melting profile of crystallization temperature. Based on the results, turbidimetry might be suggested as a fast and inexpensive method for monitoring the crystallization temperature and crystallization time for the routine crystalline fractionation process.     

The influence of chemical interesterification on physicochemical properties of complex fat systems 1. Melting and crystallization

The effects of blending palm oil (PO) with soybean oil (SBO) and lard with canola oil, and subsequent chemical interesterification (CIE), on their melting and crystallization behavior were investigated. Lard underwent larger CIE-induced changes in triacylglycerol (TAG) composition than palm oil. Within 30 min to 1 h of CIE, changes in TAG profile appeared complete for both lard and PO. PO had a solid fat content (SFC) of ∼68% at 0°C, which diminished by ∼30% between 10 and 20°C. Dilution with SBO gradually lowered the initial SFC. CIE linearized the melting profile of all palm oil-soybean oil (POSBO) blends between 5 and 40°C. Lard SFC followed an entirely different trend. The melting behavior of lard and lard-canola oil (LCO) blends in the 0–40°C range was linear. CIE led to more abrupt melting for all LCO blends. Both systems displayed monotectic behavior. CIE increased the DP of POSBO blends with ≥80% PO in the blend and lowered that of blends with ≤70% PO. All CIE LCO blends had a slightly lower DP vis-à-vis their noninteresterified counterparts.     

The effect of various dietary factors on the size distribution of lymph fat particles in rat

By means of cellulose acetate electrophoresis and measurement of radioactivity, lipoproteins (d≤1,006) of lymph collected from rats fed a diet containing fats added to labeled fatty acids for 20–24 hr, have been separated into two kinds differing in their size. Fats with different saturated and unsaturated fatty acid content were tested: corn oil, lard, mutton tallow, tripalmitin, corn oil-lard mixture, and randomized palmitic-linoleic triglycerides. Factors studied were: (a) increased amounts of these fats given alone or included in a test meal; (b) added amounts of nutrients (other than fats) in the test meal; (c) adaptation to a diet containing 20% fat for 10 days. The major part of the labeled lymph lipid was always transported by the smaller particles. Size distribution of lymph fat particles was influenced by some of the factors studied. Generally, unsaturated fats produced higher amounts of larger particles.     

Studium der UV-Spektren oxydierter Fette III

Studies on the UV-Spectra of Autoxidized Fats III The author has determined the various properties of oxidized oils and fats with relation to the first maximum of extinction E₁ according the direct UV-method (E_1cm^1%). Following fats and oils were investigated: sunflower oil, rapeseed oil, peanut oil, soybean oil, corn oil, lard, butter, beef tallow and hardened edible fat.     

Enzymatic interesterification of lard and high-oleic sunflower oil with Candida antarctica lipase to produce plastic fats

Lard and high-oleic sunflower oil (Trisun® Extra) were interesterified at 55°C for 24 h with SP435 lipase from Candida antarctica to produce plastic fats. As the amount of trisun increased, percentage free fatty acid, unsaturated fatty acid/saturated fatty acid value, oxidizability, and the amount of 18:1 found at the sn-2 position of triglyceride products increased. Differential scanning calorimetry showed that the low-melting components in the product contained more 18:1 than the high-melting components. A 60:40 (w/w) ratio of lard to trisun had the widest plastic range (3–26°C). The scaled-up reaction to produce this blend resulted in a product that had 60.1% 18:1 at the sn-2 position compared to 44.9% for the physical blend. The solid fat content of the 60:40 interesterified mixture resembled soft-type margarine oil.     

Detection of refined animal and vegetable fats in adulteration of pure milkfat

The objective of this research was to evaluate the presence of dehydroxylated sterols in samples of butter adulterated with exogenous refined fat of both animal and vegetable origin. The 3,5-cholestadiene, derived from the refining treatment, was found to be an index for the addition of refined beef tallow to butter. Moreover, several dehydroxylated phytosterols could be detected in butter adulterated with vegetable oil. The proposed method seemed to be a suitable criterion for detecting adulteration of pure butter with other fats.     

An alkali rendering process for lard and other animal fats

Summary An alkali rendering process for the production of edible animal fats has been described. Laboratory and semi-plant scale experiments indicate that high quality edible lard and beef fat may be produced in a semi-continuous process. Alkali rendered pork and beef fats are suitable for compounding into high quality domestic and commercial shorteners. Presented at 87th annual spring meeting of the American Oil Chemists’ Society in New Orleans, La., May 15–17, 1946.     

Composition and thermal profile of crude palm oil and its products

Gas-liquid chromatography and high-performance liquid chromatography (HPLC) were used to determine fatty acids and triglyceride (TG) compositions of crude palm oil (CPO), refined, bleached, and deodorized (RBD) palm oil, RBD palm olein, and RBD palm stearin, while their thermal profiles were analyzed by differential scanning calorimeter (DSC). The HPLC chromatograms showed that the TG composition of CPO and RBD palm oil were quite similar. The results showed that CPO, RBD palm oil, RBD olein, and superolein consist mainly of monosaturated and disaturated TG while RBD palm stearin consists mainly of disaturated and trisaturated TG. In DSC cooling thermograms the peaks of triunsaturated, monosaturated and disaturated TG were found at the range of −48.62 to −60.36, −25.89 to −29.19, and −11.22 to −1.69°C, respectively, while trisaturated TG were found between 13.72 and 27.64°C. The heating thermograms of CPO indicated the presence of polymorphs β₂′, α, β₂′, and β₁. The peak of CPO was found at 4.78°C. However, after refining, the peak shifted to 6.25°C and became smaller but more apparent as indicated by RBD palm oil thermograms. The heating and cooling thermograms of the RBD palm stearin were characterized by a sharp, high-melting point (high-T) peak temperature and a short and wide low-melting point (low-T) peak temperature, indicating the presence of occluded olein. However, for RBD palm olein, there was only an exothermic low-T peak temperature. The DSC thermograms expressed the thermal behavior of various palm oil and its products quite well, and the profiles can be used as guidelines for fractionation of CPO or RBD palm oil.     

Fractionation of animal fat glycerides by crystallization from acetone. Am improved lard oil

Summary Various edible and inedible grades of animal fats, such as lard, grease, tallow, and selectively hydrogenated lard, grease and tallow were separated into “oils” and “stearins” by crystallization from acetone. The chemical and physical properties as well as the yields of oils and stearins obtained by this method are described. Antioxidants and metal deactivators are much more effective in stabilizing lard and grease oils produced from partially hydrogenated fats than in stabilizing corresponding products from unhydrogenated fats. Report of a study certain phases of which were made under the Research and Marketing Act of 1946. One of the laboratories of the Bureau of Agricultural and Industrial Chemistry, Agricultural Research Administration, United States Department of Agriculture.     

Spurennachweis von mehrfach verzweigten Fettsäuren in Fetten

Detection of Traces of Polybranched Fatty Acids in Fats A method for the detection and quantitative determination of saturated polybranched fatty acids in animal and vegetable fats is described. The method is based on gas-chromatographic determination of polybranched fatty acid methyl esters in the methyl esters which do not form urea adducts. The following amounts of polybranched fatty acids were determined in animal fats: whale oil 15 000 ppm., fish oil 6000 ppm., butter fat 4000 ppm., beef tallow 2000 ppm. and lard 110 ppm. In different vegetable oils and fats upto 200 ppm. of polybranched fatty acids were found. Not only the difference in total content of polybranched fatty acids but also differences in their percentage composition and retention volumes in gas-chromatograms were found. This method therefore offers the possibility of identification of some of the animal fats.     

Comparison of four accelerated stability methods for lard and tallow with and without antioxidants

The oxidative stability of lard and tallow with and without antioxidants was evaluated by four accelerated stability methods, the active oxygen method (AOM), the oxygen bomb test, the Rancimat method, and the Schaal oven test. The results indicated that the oxidative stability of animal fats and the relative effectiveness of an antioxidant in the fats could have different mechanisms. When the protective index was used to demonstrate the relative effectiveness of the antioxidants, the results suggested that the Rancimat Method may be the least reliable method compared with AOM, oxygen bomb test, and Schaal oven test. More than one accelerated stability method is recommended for evaluating the effectiveness of an antioxidant or the oxidative stability of fats.     

Dietary fat and colon cancer: Animal model studies

Since it was first suggested that high dietary fat is a risk factor in colon cancer, there have been several studies to test this hypothesis. Epidemiologic studies suggested a positive association between dietary fat and colon cancer. Laboratory animal model studies demonstrated that not only the amount of rat, but also types of fat differing in fatty acid composition are important determining factors in colon tumor development. Chemically-induced colon tumor incidence was increased in rats fed the semipurified diets containing 23% corn oil, safflower oil, lard or beef tallow (high-fat) as compared to those fed 5% corn oil, safflower oil, lard or beef tallow diets (low-fat). Diets containing 23% conconut oil, olive oil or fish oil, or high-fat diets containing varying levels oftrans fat, had no colon tumor-enhancing effect compared to their respective low fat diets. The stage at which the effect of dietary fat is exerted appears to be mostly during the post-initiation phase of colon carcinogenesis. Lack of a colon tumor enhancing effect of dietary fish oil is observed both during the initiation and postinitiation phases. The mechanisms by which various dietary fats increase colon carcinogenesis are not fully understood. In most instances, however, the high-fat diet appears to enhance tumorigenesis through elevation of agents, such as secondary bile acids, that act as promoters of tumor development. Lack of colon tumor promotion by dietary fish oil andtrans fat appears to be mediated through their effect on mucosal ornithine decarboxylase activity, colonic secondary bile acids and/or prostaglandin synthesis. Based on a paper presented at the Symposium on Lipids in Cancer held at the AOCS Annual Meeting, Baltimore, MD, April 1990.     

On the glyceride composition of animal fats

Summary In agreement with comments of Hilditch but in contrast with certain other statements in the literature it is concluded that lard, beef tallow, and mutton tallow are non-random in distribution of fatty acid chains among their glycerides. From thermal and x-ray diffraction techniques applied to S₃, S₂U, SU₂, and U₃ fractions of these fats and to the various products of complete hydrogenation it is concluded that lard is composed largely of 2-palmityl glycerides as proposed by Hilditch while the tallows are composed largely of 1-palmityl glycerides.     

Enzymic hydrolysis of animal fats in organic solvents at temperatures below their melting points

Lipase fromCandida rugosa catalyzed the hydrolysis of inedible beef tallow and pork lard (edible and inedible) in the presence of organic solvents at temperatures below the melting point of the fat. Reactions were carried out at 50% substrate with 180 lipase units per gram of fat in a two-liter reactor. In the presence of isooctane (5-10%) beef tallow yielded 94% hydrolysis in 24 hr both at 37° and 31°C. Edible pork lard yielded 97% hydrolysis under these conditions and at temperatures as low as 25°C, while inedible lard gave hydrolysis intermediate between the other two fats.