Quality of cold-pressed edible rapeseed oil in Germany

Bertrand Matthus and Ludger Brhl

Forty-eight cold-pressed edible rapeseed oils obtained from smalland medium-sized decentralized plants located all over Germany were characterized by different chemical parameters for their composition and by descriptive sensory evaluation. Between the different oils great differences could be noticed for each parameter. The results evidenced that additionally to the features given in the Guidelines for edible fats and oils of the German Food Codex, especially the sensory evaluation, the oxidation stability (Rancimat), content and the composition of tocopherols, the content of trans-fatty acids and the content of steradienes were crucial parameters to guarantee a high-quality product for the consumer.

1 Introduction
Rapeseed is the most important oil crop in Germany today. In 2000, the cultivation came to about 1.14 Mio ha. This is about 10% of the area used as farmland in Germany. Rapeseed oil amounts to 65% of the whole quantity of edible oil produced in Germany and the consumption of rapeseed oil for nutrition came to about 560.000 t for the year 2000, without oil for export and non-food. The most important application was the production of margarine. Nearly 150.000 t were distributed in bottles for nutrition, but only a small part labelled as rapeseed oil. Only small amounts of nearly 10.000 t were sold on the market as cold-pressed rapeseed oil. The role of rapeseed oil in nutrition becomes increasingly strengthened. Different investigations have shown the excellent nutritional properties of this oil, as a result of the good balanced fatty acid composition [1, 2]. The German report of nutrition 2000 [3] gave special mention to rapeseed oil, as particularly favourable for human nutrition, even better then olive oil. In this report, it is recommended to prefer the use of rapeseed oil in the preparation of dishes, whenever possible. Above all, the content of n-3 and n-6 fatty acids was emphasized and especially the value of n-3 fatty acids for the prevention of endemic diseases such as cardiovascular diseases and inflammable rheumatic diseases, respectively, were named. Most consumers use refined oil as a universal oil in the kitchen. This has a great field of applications, because of its bland and neutral taste. Additionally, the use of cold-pressed edible oils becomes more and more popular for salads and similar preparations. The consumer appreciates especially the typical, characteristic taste, the specific aroma and the intensive colour of such cold-pressed oils. These sensory features set cold-pressed oils apart from the tasteless refined oils, but also the gentle processing of the cold-pressed oils is an important feature for consumers. In Germany, the greatest amount of oilseeds is processed in some centralized companies, but in the last 10 years the processing of oilseeds in so-called decentralized plants increases, especially in the rural areas. Nowadays, more than 140 smalland medium-sized oil mills are widespread all over Germany, whereas most of them are located in Baden-Wrttemberg and Bavaria. The processing capacity of such small plants ranges
Correspondence: Dr. B. Matthus, Federal Center for Cereal, Potato and Lipid Research, Institute for Lipid Research, P.O. Box 1705, D-48006 Mnster, Germany E-mail: matthaus@uni-muenster.de Fax: +49-(0)-251-519275 Keywords: Rapeseed oil / Trans-fatty acids /
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between 0.5 and 25 t/d [4, 5]. Many of them produce mainly oils for technical proposes, but in most cases additional edible oils for human consumption. Due to this, the supply of cold-pressed edible oils increases. In contrast to great centralized factories small- and medium-sized plants have short routes of transport and therefore small costs for transportation. This helps to economize in regional material cycles and increases the acceptance of the products by the consumers [4, 6]. Therefore, these plants are able to supply a manageable and quantitatively limited market with high-quality cold-pressed edible oils. In small- and medium-sized plants the processing for the production of coldpressed edible rapeseed oil is reduced to the indispensable steps pretreatment of the seeds, oil-pressing process, cleaning of the oil and storage of the oil. This processing leads to the extraction of the oilseeds with screw presses being the most simple possibility for the production of oil [79]. The crucial point for the production of a high-quality coldpressed rapeseed oil is the choice of high quality raw materials, an optimized oil pressing process, an immediate cleaning of the crude oil as well as an appropriate storage of the oil. If one of these points is not met, a drastically loss of quality will result [10]. This loss of quality is noticeable by different parameters, which describe the quality of the oil. First and foremost is this the sensory impression of the oil, which gets rancid, woody, straw-like, musty or fusty notes by formation of volatile degradation products or development of aroma active compounds during faulty processing. The aim of the present work was to gather an overview of the quality of cold-pressed edible oils sold on German markets.

2 Materials and methods

2.1 Materials Forty-eight cold-pressed edible rapeseed oils were obtained directly from the plants as supplied on the local market. Two refined rapeseed oils were purchased in a local supermarket. 2.2 Methods 2.2.1 Sensory evaluation The sensory evaluation of the oils was carried out according to the method DGF C II 1 (97) [11]. By defined conditions, the colour and transparency, as well as the flavour and taste of the oils, was characterized according to the sensory description form. The sensory evaluation of the oil was carried out according to a scale from 1 (inedible) to 5 (excellent). A panel with four trained tasters was used and the mean value of the investigation was given as the result.
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2.2.2 Fatty acid composition The method for gas chromatographic determination of fatty acid methyl esters (FAMEs) followed the ISO draft standard ISO/FDIS 5509 : 1997 [12]. In brief, about 12 mg of oil was solved in 1 mL of petroleum ether. 25 lL of a solution of 2 M sodium methanolate in methanol was added and the closed vial agitated vigorously for 1 min. About 20 mg of sodium hydrogen sulphate monohydrate extrapure was added. The closed vial was agitated again and then centrifuged at 5000 U/min for 1 min. The clear supernatant solution was transferred to another vial and was ready for injection. Gas chromatographic conditions: capillary column, DB-23, 60 m long, 0.32 mm ID; film thickness, 0.2 lm; temperature program: from 155 8C heated to 220 8C (1.5 8C/min), 10 min isotherm; injector 250 8C, FID 250 8C; carrier gas, 36 cm/s hydrogen; split 1 : 50, injection volume, 1 lL. 2.2.3 Peroxide value and oxidative stability The peroxide value of the oils was determined according to the method DGF C-VI 6a Part 1 (2000) [11]. The oxidative stability of the oils was tested by the Rancimat method [13, 14]. All experiments were carried out with a 743 Rancimat (Metrohm AG, Herisau, Switzerland). In brief, 3.6 g of the oil was weighed into the reaction vessel, which was placed in the heating block at 120 8C. Air flow was set at 20 L/h for all determinations. Volatile compounds released during the degradation process were collected in a receiving flask with distilled water. The conductivity of this solution was measured and recorded by the computer. The evaluation of the curve was carried out automatically by the Metrohm program. 2.2.4 Content of steradienes About 500 mg of oil dissolved in 1 mL of internal standard solution (20 lg/mL cholesta-3,5-diene in petroleum ether) was given onto a small dry-packed silica gel column of 5 g material (water content 2 g/100 g). The steradienes were eluted with 20 mL of petroleum ether and the solvent was removed by a rotary evaporator. The residue was solved in 500 lL of a mixture of tert-butylmethyl ether and acetonitrile (1 + 1 v/v) and directly used for injection onto an HPLC system equipped with a UV detector at 235 nm wavelength and an RP-18 column ODSII, 5 lm, 25 cm long, 4 mm ID. The separation was carried out by elution with a mixture of acetonitrile and tertbutylmethyl ether (7 + 3 v/v), at a flow rate of 1 mL/min and 20 lL sample volume [15]. 2.2.5 Smoke point The smoke point of the oils was determined according to the method DGF C-IV 9 (84) [11]. In brief, the sample is heated under defined conditions (Cleveland-apparatus) and the temperature at which the development of smoke was clearly visible was defined as smoke point. 2.2.6 Content of chlorophyll The content of chlorophyll was determined according to the method Cc 13i-96 of the AOCS [16]. The absorbance of the sample was measured at 630, 670 and 710 nm against air and the content calculated using the absorbtivity of pheophytin A, which is the main chlorophyll pigment in crude vegetable oils.
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3 Results and discussion

Forty-eight cold-pressed oils, as well as two refined edible rapeseed oils, were investigated regarding parameters describing the sensory impression, oxidative stability and effects of heating during the processing. These parameters are important to ensure the sensory, nutritional and healthy properties of the oil necessary to offer a high-quality product to the consumer. The present investigation was an inquiry of the market, therefore information about parameters describing the processing of the oils were not available. Thus, it is not possible to correlate certain results with parameters of the processing such as pretreatment of the raw materials, pressing procedure or cleaning and storage of the oil. 3.1 Sensory evaluation One of the most important parameters for the assessment of the quality of edible oils is the sensory evaluation. The result of the sensory evaluation can be objectified by different chemical parameters, but the sensory impression is the decisive factor for the evaluation of the oil as edible provided that no toxic contaminants are against this assessment. One reason for the importance of the sensory quality of the oil is that more than any other parameter the appearance and the taste deeply influences the buying decision of the consumer. Typical for coldpressed rapeseed oil are seed-like and nutty aroma attributes as positive attributes whereas attributes like rancid, straw-like, woody, fried, burnt, fusty, muddy, bitter and astringent belongs to the typical off-flavours. The results of the sensory evaluation of the oils are given in Fig. 1, as mean values of the results of four different tasters. Additionally, to a number of oils with a characteristic seed-like and nutty note, as to be expected for cold-pressed rapeseed oil, some of the oils showed serious sensory defects, which resulted in the classification as inedible. From a total of 48 cold-pressed oils 15 oils were classified as not sufficient and 4 oils were unsuitable for human consumption. On the other hand, for 14 oils the sensory evaluation resulted in a good or premium classification. The fact that about one-third of the investigated oils were more or less unacceptable from a sensory point of view shows that a lot of oils are available on the market, which could lead to a rejection of cold-pressed rapeseed oil by the consumers in the future. But the results show also that it is obviously possible to produce high-quality coldpressed rapeseed oils, which correspond to the expectations of the consumers. 3.2 Fatty acid composition For authentication purposes the fatty acid composition is an important feature, however, rapeseed oil as major crop in Germany is a cheap oil, which is normally not adulterated with other oils. In some cases an admixture of sunflower or soybean oil might occur. These blends might come from the great oil refining companies by switching from rapeseed processing to the processing of another crop. However, the fatty acid composition of all the oils investigated in this study varied within the common natural ranges. The content of the main unsaturated fatty acids, oleic acid, linoleic acid and a-linolenic acid, was between 50.9 and 61.5 g/100 g, 17.3 and 28.6 g/100 g, as well as 7.4 und 12.4 g/100 g, respectively (Fig. 2). This demonstrates that all these fatty acids include a great breeding potential, because there was a remarkable variation in the amounts of the fatty acids between the different rapeseed oils.
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Quality of rapeseed oil

Figure 1. Sensory assessment of the cold-pressed rapeseed oils according to the DGF-method CII 1 (97) with 5 for an excellent oil and 1 for an oil not suitable for human nutrition.

Figure 2. Average fatty acid composition of cold-pressed rapeseed oils from the German market. The variation within the different samples is given as black bars.

The total amount of the main saturated fatty acids, palmitic acid and stearic acid, had an average of 6.3 g/100 g, with a variation from 5.5 to 7.7 g/100 g, which presents these characteristic features as very stable. This is interesting especially from a nutritional point of view, since the saturated fatty acids are reputed to be responsible for adverse effects on serum lipoproteins and apolipoproteins, which cause cardio-vascular diseases [17, 18]. One constituent which could lower the nutritional value of rapeseed oil is erucic acid. Thirty years ago, rapeseed oil contains more than 50% of the total fatty acids as erucic acid which produce cardiac fat droplets resulting in myocardial lipiosis [19, 20]. Nowadays, the content of erucic acid is limited to 5% by the Erucic Acid decree and the Codex Alimentarius prescribes a maximum of 2% erucic acid in rapeseed oil [21, 22]. As a result of plant breeding programs, the content of erucic acid in the oil was drastically reduced, so that in most cases the amount in the oils investigated in this paper was well below the limit given by the Codex Alimentarius (Fig. 2). The content varied between 0.04 and 2.17 g/100 g, with an average of 0.37 g/100 g. Only two oils show higher amounts of erucic
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acid than 1 g/100 g, which indicates that today it should be no problem to produce rapeseed oil with very low amounts of this fatty acid. 3.3 Oxidation Oxidation is the main cause of oil deterioration. Primary products of the lipid oxidation are hydroperoxides, which result in the formation of short-chain, sensory-active compounds. In most cases, the sensory impression caused by these compounds is undesirable, because the oils get a rancid and scratchy aroma. Further on, oil with a high level of hydroperoxides is less stable against oxidative degradation, even if undesirable aroma compounds are still not obvious. The oxidation state of the oils is described by the peroxide value which registers the peroxidic bonded oxygen in the oil. The speed of the lipid oxidation is strongly influenced by different factors such as temperature during processing and storage, oxygen availability, water activity, exposure to light, presence of antioxidants or pro-oxidants, etc. which in most cases can be attributed to an improper treatment during processing and storNahrung/Food 47 (2003) No. 6, pp. 413 419 415

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Figure 3. Peroxide values of cold-pressed rapeseed oils from the German market. Samples with numbers 36 and 47 were refined oils.

Figure 4. Oxidative stability of the rapeseed oils measured by the Rancimat method at 120 8C. Samples with numbers 36 and 47 were refined oils.

age. Prerequisite for a long-term storage stability, which has some importance for the consumer of the oils, is a low peroxide level after the processing, although the peroxide value alone is no measure for state and storage stability of oil. Figure 3 shows a wide range of peroxide values for the different oils, which varied between 0.1 and 13.9 meqO2/kg. Regarding the Guidelines of the German Food Codex oils which contain more than 10.0 meqO2/kg has to be classified as inedible. Four cold-pressed oils exhibited a higher peroxide value than the limit given in the Guidelines. For further 15 oils the peroxide value was in the range between 5 and 10 meqO2/kg, which indicates a significant oxidative damage of these oils during processing or storage. On the other hand, the investigation shows also that it is possible to produce cold-pressed rapeseed oil with low amounts of peroxides, which can ensure a long-term storage before consumption. Additionally to the oxidation state of the oils, which gives some indications about a careful processing, the oxidative stability, measured by the Rancimat method at 120 8C, can show any oxidative damage of the oil during processing. The results of this method allow no direct conclusions on the storage ability of the oils under homemade conditions, but it is possible to compare the oxidative stability of different oils under similar conditions. It can be
416 Nahrung/Food 47 (2003) No. 6, pp. 413 419

expected that oils with a high stability in the Rancimat test will also show a higher stability during storage under household conditions. The stability of the oils under the conditions given by the Rancimat method varied between 40 min and 5 h 44 min, with an average stability of 3 h 34 min (Fig. 4). Surprisingly, not the refined oils (Nos. 36 and 47) but some of the cold-pressed edible rapeseed oils showed the highest oxidative stability in the Rancimat test. Furthermore, the results show that at least four oils experienced an oxidative deterioration during the storage of the seeds, the processing of the oil or the storage of the oil. The oxidative stability of these oils was very low (about 1 h) in comparison to the other oils under the conditions of the Rancimat method. Additionally, it is obvious that it is possible to produce coldpressed rapeseed oil with a high oxidative stability as presented by six oils with induction periods nearby or higher than 5 h. A further factor strongly influencing the oxidative stability of oils is the content of chlorophyll, especially if the oils are exposed to light. Furthermore, chlorophyll is undesirable because it results in an unpleasant green or brown colour of the oil. Chlorophyll is a ubiquitous plant pigment, which is described in literature as a photosensitizer for singlet oxygen formation under light which results in a faster deterioration of
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Quality of rapeseed oil

Figure 5. Content of chlorophyll of coldpressed rapeseed oils from the German market. Samples with numbers 36 and 47 were refined oils.

Figure 6. Content of steradienes of coldpressed rapeseed oils from the German market. Samples with numbers 36 and 47 were refined oils.

the oil [23]. Above all, the content of chlorophyll is a measure of maturity for the raw material, but it also gives indications to the application of improper pressing conditions. The more drastic the pressing conditions the higher the content of chlorophyll in the resulting oil. Additionally a higher content of chlorophyll indicates the processing of broken, sprouted or frosted seed material during the oil pressing process, because in such seeds an increased amount of chlorophyll can be found [24]. The amount of chlorophyll in the oils varied from 0.3 to 174.5 mg/kg with an average of 43.6 mg/kg (Fig. 5). In most of the oils (78%), the content of chlorophyll was higher than 20 mg/kg and lower than 60 mg/kg. To avoid a rapid oxidation of the oil in the presence of light a concentration of chlorophyll lower than 50 mg/kg is necessary [25]. Using the Canadian trading specification for Canola quality it is recommended that the crude oils should contain a maximum of 30 mg/kg chlorophyll [26], which was met by 20 oils. 3.4 Heat treatment during processing A proof for an improper processing of cold-pressed edible oils can be done by the investigation of the content of transfatty acids or the determination of stigmasta-3,5-diene. Transfatty acids are formed at temperatures higher than 190 8C duri 2003 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim

ing steam washing of oils, but also during an extensive heating at the drying process of the raw materials. Stigmasta-3,5-diene is developed from natural occurring b-sitosterol as the result of a treatment of oils with bleaching earth or a deodorising process. Therefore, both parameters are useable for the assessment of an adulteration of cold-pressed oils with refined oils or an improper processing of cold-pressed oils. Figure 6 shows that not only the refined oils Nos. 36 and 47 had higher contents of steradienes. For cold-pressed oils, besides olive oil no limit for the content of steradienes is defined, but for the differentiation of refined from cold-pressed olive oil the maximum limit is prescribed for 0.15 mg/kg [27]. However, also for other cold-pressed oils it seems to be possible to use this limit for an assessment of the processing quality of the oils. Normally the content of steradienes in cold-pressed oils does not exceed 0.05 mg/kg [28]. From this it could be established that 17 oils exceed the limit of 0.05 mg/kg, but only in four cold-pressed oils higher amounts of steradienes than 0.15 mg/kg were found, which indicated an adulteration with refined oil or an improper processing in which course the raw material or the oil got too hot. The other important parameter for the detection of an improper processing of cold-pressed oils or an adulteration with refined oils is the determination of the trans-fatty acids, which
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Matthus and Brhl

Figure 7. Content of trans-fatty acids of cold-pressed rapeseed oils from the German market. Samples with Nos. 36 and 47 were refined oils.

naturally occur only in small amounts in cold-pressed oils. Trans-fatty acids are formed during drying of seeds after harvest at higher temperatures, but also at deodorization with temperatures above 150 8C during the refining process. Most of the oils showed amounts of trans-fatty acids between 0.1 and 0.2 g/100 g, with an average of 0.18 g/100 g (Fig. 7). As expected, the highest amounts were found for the two refined oils with 0.5 and 0.83 g/100 g, respectively. Only three other oils had contents of trans-fatty acids higher than 0.2 g/100 g, with 0.21, 0.29 and 0.48 g/100 g, respectively. From this it can be assumed that cold-pressed rapeseed oils with higher amounts of trans-fatty acids than 0.2 g/100 g have been exposed to improper conditions during the processing. Therefore, this parameter seems to be suitable to characterise coldpressed oils as really cold-pressed products. From the results of trans-fatty acids and steradienes it is obvious that only oil No. 22 shows high values for both of these methods. For the other oils a correlation between the amount of trans-fatty acids and steradienes is not given. One reason is that the sterols are more susceptible against heat treatment and therefore a formation of steradienes is faster than the formation of trans-fatty acids.

essential to introduce a quality standard in the field of coldpressed edible rapeseed oil. Furthermore, the results show that it is possible to produce cold-pressed edible oils of high quality, which will be accepted by the consumer and which correspond to the demand for a natural product. From virgin olive oil it can be learned, that the quality of a product can reach a high level by setting up a quality standard, which will be rewarded by the consumer. Only the introduction of such a standard, which guarantees a constant high quality, leads to a successful establishment of cold-pressed edible rapeseed oil on the market.

5 References
[1] Trautwein, E. A., Rieckhoff, D., Kunath-Rau, A., Erbersdobler, H. F., Ann. Nutrit. Metab. 1999, 43, 159172. [2] Royal Swedish Academy of Science, Scand. J. Nutrit. 1993, 37, 4971. [3] German Nutrition Report 2002, Druckerei und Verlag Henrich GmbH, Frankfurt/Main. [4] Widmann, B. A., Forschungsbericht Agrartechnik. MEG Nr. 262, Institut fr Landtechnik Weihenstephan 1994. [5] Shukla, V. K. S., Blicher-Mathiesen, U., Fat Sci. Technol. 1993, 95, 367369. [6] Widmann, B. A., in: Landwirtschaft und Forsten, Bayer. Staatsministerium fr Ernhrung, Forschungsbericht, Mnchen 1994. [7] Peterson C. L., Auld, D. L., Thompson, J. D., Transact. ASAE 1983, 5, 12981302. [8] Stver, H.-M., Mnch, E.-W., Sitzmann, W., Fat Sci. Technol. 1988, 90, 547550. [9] Dunning, J. W., J. Am. Oil Chem. Soc. 1953, 30, 486492. [10] Niewiadomski, H., in: Niewiadomski, N. (Ed.), Rapeseed Chemistry and Technology, Elsevier, Amsterdam 1990, pp. 123 160. [11] German Standard Methods, Wissenschaftliche Verlagsgesellschaft, Stuttgart 2001. [12] ISO/DIS 5509:1998, Animal and vegetable fats and oils Preparation of methyl esters of fatty acids. [13] Metrohm Application Bulletin Nr. 204/1 d 1994. [14] Lubli, M. W., Bruttel, P. A., J. Am. Oil Chem. Soc. 1986, 63, 792795. [15] Brhl, L., Fiebig, H.-J., Fat Sci. Technol. 1995, 97, 203208. [16] Official Methods and Recommended Practices of the American Oil Chemist's Society (AOCS), Champaign, IL, USA 1990.
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4 Concluding remarks
The results presented in this paper demonstrate that in addition to the parameters given by the Guidelines for edible fats and oils of the German Food Codex especially the sensory properties, the oxidative stability (Rancimat test), as well as the content of trans-fatty acids and stigmasta-3,5-diene were of importance for an assessment of the quality of cold-pressed edible rapeseed oil. The rapeseed oils available on the market differ markedly in their quality. This can be explained by the reason that each producer defines his own quality criteria within the scope of the legislative recommendations. In some plants the oil is even pressed without any deeper knowledge of the context and own quality controls are not always carried out. From this it follows for the consumer that it is impossible for him to judge, if he buys a cold-pressed edible rapeseed oil produced with utmost care from high-quality raw materials or not. For a greater transparency in this point, it is absolutely
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Quality of rapeseed oil [17] [18] [19] [20] Weber, N., Getreide, Mehl und Brot 2001, 55, 111119. Zllner, N., Tatu, F., Clin. Investig. 1992, 70, 9681009. Beare-Rogers, J. L., Nera, E. A., Lipids 1972, 7, 4650. Sauer, F. D., Kramer, J. K. G., in: Kramer, J. K. G., Sauer, F. D., Pigden, W. J. (Eds.), High and Low Erucic Acid Rapeseed Oil Production, Usage, Chemistry and Toxicological Evaluation, Academic Press, New York 1983, p. 260. [21] Deutsches Lebensmittelbuch: Leitstze 2000, Bundesanzeiger, 1999, pp. 303315. [22] Draft Codex Standard for Named Vegetable Oils (ALINORM 97/ 17), Joint FAO/WHO Food Standard Programm 1997. [23] Fakourelis, N., Lee, E. C., Min, D. B., J. Food Sci. 1987, 52, 234235. [24] Daun, J. K., Burch, L. D., J. Am. Oil Chem. Soc. 1984, 61, 1117 1122. [25] Mag, T. K., in: Erickson, D. (Ed.), Edible Fats and Oils Processing: Basic Principles and Modern Practices, The American Oils Chemists Society, Champaign, IL 1989, pp. 107116. [26] DeClercq, D. R., Daun, J. K., Canadian Grain Commission 2001. [27] Verordnung (EG) Nr. 796/2002 vom 6. Mai 2002, Amtsblatt der Europischen Gemeinschaften. [28] Grob, K., Biedermann, M., Artho, A., Schmid, J. P., Riv. Ital. sost. Grasse 1994, 71, 533538. Received May 2, 2003 Accepted July 8, 2003

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