PH/RB Foodproc. 01

29-03-2001

Pagina 1

HR 7600/1 Comfort

HR 2831/6 Cucina

HR 2833/6 Cucina

HR 7633/6 Cucina

HR 7638/6 Cucina

HR 7720/6 Cucina

HR 7725/6 Cucina

HR 7727/6 Cucina

Foodprocessor range 2001

FOODPROCESSORS

ACCESSORIES

HR 7600/1 Features

HR 2831/6

HR 2833/6

HR 7633/6

HR 7638/6

HR 7720/6

HR 7725/6

HR 7727/6
Metal blade Rev. slicing/grating disc
Wattage Speeds Bowl capacity dry (L) Bowl capacity liquid (L) Blender jar capacity max. (L) Flour for yeast dough (gr) Suction cups Cordstorage Overload protection Accessories Metal blade Slicing insert fine Slicing insert medium Shredding insert fine Shredding insert medium Shredding insert coarse Granulating insert Rev. slicing/grating disc Rev. slicing disc Rev. grating disc (medium/coarse) Rev. grating disc (fine/very fine) French fries disc (HR 2912) Balloon beater Plastic kneading knife Emulsifying disc Metal kneader Blender jar Storage Citrus press Juice extractor Fruitfilter Pusher Spatula Recipes
q q P V = = = = = Standard Optional Not available Pulse position Vario speed
350 1+P 2,1 1,5 rubberring

350 2+P 2,2 0,

350 V+P 2,2 0,

450 2+P 1,8 1,2 1,25

700 2+P 2,5 1,0

700 2+P 2,5 1,0 2,0

700 V+P 2,5 1,0 2,0
Rev. slicing disc Rev. grating disc (medium/coarse) Rev. grating disc (fine/very fine) French fries disc (HR 2912) Balloon beater Plastic kneading knife
400 (0,96 kg dough) 400 (0,96 kg dough) 700 (1.2 kg dough) 700 (1.2 kg dough) 700 (1.2 kg dough)

q q q q q q q

q q q q q q q q q q q q

Microstore

q q q q q q q q q q q q q
Metal kneader Blender jar Storage box for discs Citrus press Juice extractor Double pusher Recipes Slicing insert fine Slicing insert medium Schredding insert fine Schredding insert medium Schredding insert coarse Granulating insert Emulsifying disc Spatula
q (box for discs) q q q q q q
q q (box for discs) q q q q q q
q q (box for discs) q q q q (double) q q

Microstore

q q q q
International range (note: not all models will be available in all countries)

Fruit filter

Pagina 2
APPLICATIONAL COMPARISON FOODPROCESSING (INCLUSIVE KITCHENMACHINE) STANDARD VERSIONS

LOGISTIC DATA

HR 7600/1 Functions Kneading Creaming Mixing Emulsifying Pureeing Beating Whisking Whipping Blending Liquidizing Chopping Slicing Shredding Chipping (french fries) Shaking Crushing Crumbling Citruspressing Juice-extracting q

HR7725/6

Version
Dimensions product LxWxH (mm) 230 x 180 x x 200 x x 200 x 250 366.7 x 197.4 x 305.9 420.3 x 197.4 x 395.x 185 x x 195 x x 195 x 430
Dimensions packaging LxWxH (mm) 280 x 195 x x 280 x x 280 x x 248 x x 248 x x 273 x x 273 x x 273 x 510
Weight Pieces complete per unit f-box (grams) 1 1

Pallet Phil./ euro 45 36

EAN code CTV 87 10103.

q

HR 7600/1 HR 2831/6 HR 2833/6 HR 7633/6 HR 7638/6 HR 7720/6 HR 7725/6 HR 7727/6

125181 125242

883772560 883772760
q = Optional = Not available
= Less suitable = Suitable = Very suitable
Product specification is subject to change without prior notice. For concern use only. D.A.P. Division, Groningen, Holland.

EUROPEAN COMMISSION

JOINT RESEARCH CENTRE Institute for Reference Materials and Measurements Food Safety and Quality Unit B-2440 Geel (Belgium)
Validated Method Method Description for the Detection of Cocoa Butter Equivalents in Cocoa Butter and Plain Chocolate
Manuela Buchgraber, Elke Anklam

EUR 20742 EN

Scope and Field of Application
This Standard specifies a validated procedure for the detection of cocoa butter equivalents (CBE) in cocoa butter (CB) and plain chocolate by high-resolution capillary gas chromatography (HR-GC) of triglycerides and subsequent data evaluation by regression analysis. The method has been validated for the detection of 2% CBE admixture to cocoa butter corresponding to about 0.4% in chocolate (assumed fat content of chocolate 20%).

Principle

Cocoa butter, or the fat obtained by solvent extraction from plain chocolate, is separated by HR-GC into triglyceride fractions according to their molecular weight and degree of unsaturation. The presence of CBEs is detected by linear regression analysis applied to individual triglyceride fractions of the fat analysed.

Reagents and Materials

All reagents shall be of recognised analytical grade, unless otherwise stated. 3.1 Fat solvent (non-chlorinated solvents e.g. ether, n-heptane, iso-octane) 3.2 Cocoa butter, Certified Reference Material (CRM) IRMM-801, for calibration purposes and system suitability check

Apparatus

4.1 Balance, sensitivity 1 mg 4.2 Volumetric flasks, of capacity 20 mL 4.3 Pipettes, of capacity 1 mL 4.4 Drying oven, maintained at 55 C (dry heater block may be used) 4.5 Gas chromatograph (GC): a chromatograph fitted with a cold on-column injection system and a flame ionisation detector (FID). (Note: alternative injection system, e.g. a split injector, a programmed-temperature vaporizer (PTV) or a moving-needle injector, may be used provided the same results are obtained as indicated in 8.1) The separation and detection have proven to be satisfactory if the following experimental conditions are followed: - GC column: 25 - 30 m x 0.25 i.d. fused silica coated with thermo stable 50% phenylmethylpolysiloxane to a film thickness of 0.1 0.15 mm (Note: Suitable columns are listed in Annex A, Table A.1) - temperature programme: 100 C (initial temperature), programme rate 30 C/min to 340 C (final temperature). (Note: Operating conditions may be changed to obtain optimum separation of cocoa butter triglycerides) - carrier gas: helium or hydrogen (purity 99.999%) Alternative experimental conditions, used in an international collaborative study, are listed in Annex A, Table A.1. 4.6 Chromatographic data system 4.7 Micro syringe: maximum volume 10 ml, graduated to 0.1 ml. (Note: an automatic sampler may be used)
4.8 Food grater: a kitchen blender with a design featuring the motor above the receiving container to avoid melting the samples (e.g. Philips HR2833)
Preparation of cocoa butter CRM for calibration purposes and system suitability check
Before opening and using the cocoa butter CRM (3.2), the ampoule has to be warmed in a drying oven (4.4) until the contents have melted. When a clear solution is obtained, mix the contents by repeated inversion for not less than 20 sec., open and transfer the contents to a clean vial, which can be tightly sealed and preserved in a cool place for future usage.
Preparation of the test sample
According to AOAC Official Method 970.20 [1] chill ca 200 g chocolate until hard, and grate to fine granular condition using a mechanical device (4.8). Mix thoroughly and preserve in tightly stoppered bottle in a cool place.

Procedure

7.1 Fat extraction Obtain the fat from the chocolate prepared as described in (6) according to the AOAC Official Method 920.75 [2]. That is to say, fat is separated from g grated chocolate by extracting with two or three 100 mL portions of ether. (Note: alternative extraction procedures may be used, e.g. by Soxhlet, by supercritical carbon dioxide or by using microwaves, provided that the same results are obtained). 7.2 Separation of individual triglycerides by HR-GC The test samples (cocoa butter, fat extracted from chocolate, cocoa butter CRM (3.2)) have to be warmed in a drying oven (4.4) until completely melted. If the liquid sample contains sediment, filter the sample inside the oven to obtain a clear filtrate. Pipettes (or similar equipment) used for transferring the sample during weighing operations should be brought to a temperature of ca 55 C in a drying oven in order to avoid partial fat fractionation. Weigh ca 0.2 g test sample in a 20 mL volumetric flask (4.2) and bring to volume with a suitable fat solvent (3.1). Pipette 1 mL of the resulting solution in another 20 mL volumetric flask and bring to volume with the same solvent. Inject 0.5-1.0 ml of the final test solution (0.5 mg fat/mL) into the HR-GC system using the cold on-column injection system. (Note: alternative sample amounts and injectors may be used provided that the detection system employed gives a linear response and the system suitability criteria (8.1) are met). 7.3 Identification Identification of the five major triglyceride fractions 1,3-dipalmitoyl-2-oleoylglycerol (POP), 1palmitoyl-2-oleoyl-3-stearoylglycerol (POS), 1-palmitoyl-2,3-dioleoyl-glycerol (POO), 1,3distearoyl-2-oleoylglycerol (SOS), and 1-stearoyl-2,3-dioleoyl-glycerol (SOO) is made by comparison of the retention times of the test samples with those of the cocoa butter CRM (3.2). The elution order of the triglycerides of the cocoa butter CRM is given in the example chromatogram (Annex A, Figure A.1).

7.4 Calculation 7.4.1 Determination of response factors Determine the response factors of the triglycerides POP, POS, POO, SOS and SOO by injection of the cocoa butter CRM solution using experimental conditions identical to those used for the samples. Calculate the area percentage for each of the five triglyceride fractions by:

AR i [%] =

AR i 100 AR i

[Equation 1]

MR i [%] AR i [%]

[Equation 2]

ARi. area under the peak corresponding to triglyceride i in the cocoa butter CRM ARi. sum of the areas under the peaks attributed to POP, POS, POO, SOS, SOO in the cocoa butter CRM MRi [%].. mass-% of triglyceride i in the cocoa butter CRM as given in the Certificate [3] ARi [%].. area-% of triglyceride i in the cocoa butter CRM RFi detector response factor of triglyceride i in the cocoa butter CRM. 7.4.2 Calculation of weight percentages of triglycerides Calculate the weight percentage of the triglycerides POP, POS and SOS in the test sample by

MSi [%] =

RFi ASi 100 (RFi ASi )

[Equation 3]

ASi. area under the peak corresponding to the triglyceride i in the test sample RFi. response factors as determined in 7.4.1 MSi [%].. mass-% of triglyceride i in the test samples. 7.4.3 Decision if sample is pure cocoa butter The variability of the triglyceride composition is expressed by Equation 4 using the normalised triglycerides, i.e. %POP+%POS+%SOS=100% as determined in Equation 3: POP = 43.734 0.733 x SOS (residual standard deviation = 0.125) [Equation 4]
This equation was established by using a standardised data base of the triglyceride profile of 74 individual genuine cocoa butters evaluated and in-house validated by the authors. The cocoa butter CRM (3.2) was used to standardise the applied analytical methodology for the determination of the triglyceride profile of the cocoa butters.
For 99% of all analyses, pure cocoa butter complies with: POP < 44.025 0.733 x SOS [Equation 5]
A greater value of POP, as given by Equation 5, means that the sample is not pure cocoa butter.

Notes on Procedure

The details of the chromatographic procedure depend, among other factors, on the equipment, the type, age, and supplier of the column, the means of introduction of the test solution, the sample size, and the detector. Different column lengths and brands may be used, and injection volumes may be varied, if the requirements of the system suitability tests (8.1) are met. 8.1 System suitability The cocoa butter CRM (3.2) has to be used to check the suitability of the separation system. 8.1.1 Resolution The HR-GC separation system must be capable of separating the critical pairs POS/POO and SOS/SOO with a chromatographic resolution of at least 1.0. In case of failure, the chromatographic conditions (e.g. sample size, column temperature, carrier gas flow, etc) have to be optimised. 8.1.2 Determination of detector response factors Experience has shown that for a properly functioning chromatographic system the response factors for the five main triglycerides (POP, POS, POO, SOS, SOO) vary within a range of 0.8 1.2.

Validation data

The analytical approach was validated in a European collaborative study with 13 participants [4]. The results derived from this interlaboratory test demonstrate that the procedure performs well with a detection limit of at least 2% CBE admixture to CB corresponding to 0.4% CBE in chocolate (assumed fat content of chocolate 20%) without giving false-positive or false-negative results. Note: As an aid to verify the proper functioning of the chromatographic system precision data for the three triglycerides POP, POS and SOS (normalised to 100%) are given below. Details of the collaborative study on the precision of the method are listed in Annex A, Tables A.2 to A.5. 9.1 Repeatability The absolute difference between two single test results found on an identical test material by one operator using the same apparatus within the shortest feasible interval will exceed the repeatability limits r for individual triglycerides in not more than 5% of the cases. For POP values ranging from 18.99 to 25.37 g/100 g: r = 0.514 g/100 g
For POS values ranging from 43.76 to 47.73 g/100 g: For SOS values ranging from 30.87 to 33.80 g/100 g: 9.2 Reproducibility
r = 0.293 g/100 g r = 0.621 g/100 g
The absolute difference between two single test results on an identical test material reported by two laboratories will exceed the reproducibility limits R for individual triglycerides in not more than 5% of the cases. For POP values ranging from 18.99 to 25.37 g/100 g: For POS values ranging from 43.76 to 47.73 g/100 g: For SOS values ranging from 30.87 to 33.80 g/100 g: r = 0.741 g/100 g r = 0.588 g/100 g r = 0.782 g/100 g
Note: Weight percentage data for the three major fractions POP, POS and SOS of the test sample have to be calculated and normalised to 100%. Repeatability limits r and reproducibility limits R for individual triglycerides derived from this collaborative study may be applicable to mean values beyond the given range.

Reference:

[1] Official Methods of Analysis of AOAC International (1995). AOAC Official Method 970.20 Cacao Products. Preparation of Sample. [2] Official Methods of Analysis of AOAC International (1995). AOAC Official Method 920.75 Separation of Fat in Cacao Products. [3] R. Koeber, M. Buchgraber, F. Ulberth, R. Bacarolo, A. Bernreuther, H. Schimmel, E. Anklam, J. Pauwels (2003) The certification of the content of five triglycerides in cocoa butter (in press). [4] M. Buchgraber, E. Anklam (2003). Validation of a method for the detection of cocoa butter equivalents in cocoa butter and plain chocolate. Report on the validation study. EUR 20685 EN, ISBN 92-894-5510-1.

Annex A (informative)

Table A. 1: Suitable GC conditions to be used for triglyceride analyses of cocoa butter
Method possibility Column characteristics stationary phase length [m] i.d. [mm] film thickness [m] Temperature mode - oven injection temperature [C] / hold time [min] programme rate 1 [C/min] temperature 1 [C] / hold time [min] programme rate 2 [C/min] temperature 2 [C] / hold time [min] programme rate 3 [C/min] final temperature [C] / hold time [min] - injector temperature [C] - detector temperature [C] Injection mode Carrier gas type pressure [kPa] flow [mL/min] Sample concentration [mg/mL] volume injected [l] Method possibility Column characteristics stationary phase length [m] i.d. [mm] film thickness [m] Temperature mode - oven injection temperature [C] / hold time [min] programme rate 1 [C/min] temperature 1 [C] / hold time [min] programme rate 2 [C/min] temperature 2 [C] / hold time [min] programme rate 3 [C/min] final temperature [C] / hold time [min] - injector temperature [C] - detector temperature [C] Injection mode Carrier gas type pressure [kPa] flow [mL/min] Sample concentration [mg/mL] volume injected [l] 1 DB-17HT 30 0.25 0./ 300 / 350 / 30 oven track 360 OCI H2 0.8 0.3 0.RTx-65TG 30 0.25 0./ 360 / 390 split H10 0.CB-TAP 25 0.25 0./ 0.350 /21 oven track 360 OCI H15 0.RTx-65TG 30 0.25 0./ 360 / 370 split H50 0.DB-17HT 30 0.25 0./ 300 / 340 / 2 0./360 OCI H0.5 0.CB-TAP 25 0.25 0./ 320 / 360 / 370 split H12.5 0.CB-TAP 25 0.25 0./320 / 360 / 10 65-220-OCI He 90 1-2 0.RTx-65TG 30 0.25 0./ 0.330 / 350 /5 oven track 355 OCI He 0.8 0.3 0.CB-TAP 25 0.25 0./ 300 / 340 / 360 OCI H0.5 0.CB-TAP 25 0.25 0./ 360 / 360 split He 11 CB-TAP 25 0.25 0./ 350 / hot OCI H2 2.4 0.65 0.3

Retention time [min]

Figure A. 1: Triglyceride profile of the cocoa butter CRM Peak identification: 1, PPP; 2, MOP; 3, PPS; 4, POP; 5, PLP; 6, unidentified; 7, PSS; 8, POS; 9, POO; 10, PLS; 11, PLO; 12, unidentified; 13, SSS; 14, SOS; 15, SOO; 16, SLS + OOO; 17, SLO; 18, unidentified; 19, unidentified; 20, SOA; 21, AOO Experimental conditions: GC column: 25 m x 0.25 mm fused silica capillary column coated with 0.1 m Chrompack TAP Oven temperature 100 C held for min, 30 C/min to 340 held for 35 min Injector Cold on-column Detector (FID) 360 C Carrier gas H2 at 1.6 bar head pressure Amount injected 0.5 l of a 0.4 mg/mL solution Abbreviations: PPP: tripalmitin MOP: 1-margaroyl-2-oleoyl-3-palmitoylglycerol PPS: 1,2-dipalmitoyl-3-stearoylglycerol POP: 1,3-dipalmitoyl-2-oleoylglycerol PLP: 1,3-dipalmitoyl-2-linoleoylglycerol PSS: 1-palmitoyl-2,3-distearoylglycerol POS: 1-palmitoyl-2-oleoyl-3-stearoylglycerol POO: 1-palmitoyl-2,3-dioleoylglycerol PLS: 1-palmitoyl-2-linoleoyl-3-stearoylglycerol PLO: 1-palmitoyl-2-linoleoyl-3-oleoylglycerol SSS: tristaerin SOS: 1,3-distearoyl-2-oleoylglycerol SOO: 1-stearoyl-2,3-dioleoylglycerol SLS: 1,3-distearoyl-2- linoleoyl glycerol OOO: triolein SLO: 1- stearoyl -2-linoleoyl-3-oleoylglycerol SOA: 1-stearoyl-2-oleoyl-arachidoylglycerol AOO: 1-arachidoyl-2,3- dioleoylglycerol

Table A. 2: Precision data pure cocoa butter samples
pure CB (1) Year of collaborative study Number of laboratories Number of outliers Number of accepted results Mean value (g/100 g) Repeatability standard deviation sr, g/100 g Repeatability relative standard deviation RSDr, % Repeatability limit r [r = 2.8 x sr], g/100 g Reproducibility standard deviation sR, g/100 g Reproducibility relative standard deviation RSDR, % Reproducibility limit R [R = 2.8 x sR], g/100 g POP 12 20.40 0.06 0.3 0.16 0.14 0.7 0.40 POS 12 47.73 0.06 0.1 0.16 0.11 0.2 0.30 SOS 12 31.87 0.09 0.3 0.26 0.17 0.5 0.47 pure CB (2) 2002 POP POS SOS 12 19.49 47.42 33.09 0.07 0.09 0.10 0.4 0.2 0.3 0.19 0.27 0.27 0.08 0.15 0.17 0.4 0.3 0.5 0.23 0.41 0.46 pure CB (3) POP 12 18.99 0.09 0.5 0.26 0.12 0.6 0.34 POS 12 47.21 0.08 0.2 0.24 0.09 0.2 0.25 SOS 12 33.80 0.15 0.5 0.43 0.17 0.5 0.47
(1) Country origin: Grenada (2) Country origin: Ghana (3) Country origin: Ivory Coast
Table A. 3: Precision data real chocolate samples
chocolate [CBE added] Year of collaborative study Number of laboratories Number of outliers Number of accepted results Mean value (g/100 g) Repeatability standard deviation sr, g/100 g Repeatability relative standard deviation RSDr, % Repeatability limit r [r = 2.8 x sr], g/100 g Reproducibility standard deviation sR, g/100 g Reproducibility relative standard deviation RSDR, % Reproducibility limit R [R = 2.8 x sR], g/100 g POP 11 25.37 0.13 0.5 0.36 0.26 1.0 0.74 POS 11 43.76 0.10 0.2 0.28 0.21 0.5 0.59 SOS 11 30.87 0.18 0.6 0.50 0.20 0.6 0.POP 12 19.74 0.09 0.5 0.25 0.12 0.6 0.34 POS 12 47.40 0.07 0.1 0.20 0.11 0.2 0.30 SOS 12 32.86 0.07 0.2 0.21 0.11 0.3 0.31 chocolate [no CBEs added]
Table A. 4: Precision data cocoa butter with ca 2% CBE admixture
2.06% CBE/CB (1) Year of collaborative study Number of laboratories Number of outliers Number of accepted results Mean value (g/100 g) Repeatability standard deviation sr, g/100 g Repeatability relative standard deviation RSDr, % Repeatability limit r [r = 2.8 x sr], g/100 g Reproducibility standard deviation sR, g/100 g Reproducibility relative standard deviation RSDR, % Reproducibility limit R [R = 2.8 x sR], g/100 g POP 13 20.61 0.18 0.9 0.51 0.19 0.9 0.54 POS 13 47.08 0.10 0.2 0.27 0.13 0.3 0.37 SOS 13 32.31 0.22 0.7 0.62 0.25 0.8 0.70 1.98% CBE/CB (2) 2.04% CBE/CB (3) 2002 POP POS SOS POP POS SOS 19.94 46.80 33.27 19.70 46.62 33.68 0.05 0.3 0.14 0.12 0.6 0.33 0.07 0.1 0.20 0.09 0.2 0.25 0.08 0.2 0.23 0.18 0.5 0.51 0.09 0.5 0.26 0.11 0.6 0.32 0.06 0.1 0.18 0.14 0.3 0.40 0.14 0.4 0.38 0.15 0.4 0.42 2.09% CBE/CB (4) POP 12 19.86 0.03 0.1 0.08 0.09 0.5 0.26 POS 12 46.65 0.08 0.2 0.23 0.12 0.3 0.33 SOS 12 33.50 0.08 0.2 0.22 0.18 0.6 0.52

(1) CB from Grenada mixed with CBE type PMF/(Shea + Illip) [35/65] (2) CB from Ghana mixed with CBE type PMF/Shea [50/50] (3) CB from Ivory coast mixed with CBE type PMF/Sal/Mango [50/25/25] (4) CB from Ivory coast mixed with CBE type PMF/Shea/Illip [50/25/25]
Table A. 5: Precision data cocoa butter with ca 4% CBE admixture
4.05% CBE/CB (1) Year of collaborative study Number of laboratories Number of outliers Number of accepted results Mean value (g/100 g) Repeatability standard deviation sr, g/100 g Repeatability relative standard deviation RSDr, % Repeatability limit r [r = 2.8 x sr], g/100 g Reproducibility standard deviation sR, g/100 g Reproducibility relative standard deviation RSDR, % Reproducibility limit R [R = 2.8 x sR], g/100 g POP 13 20.75 0.14 0.7 0.39 0.16 0.8 0.44 POS 13 46.34 0.08 0.2 0.22 0.18 0.4 0.51 SOS 13 32.91 0.17 0.5 0.48 0.28 0.8 0.78 3.96% CBE/CB (2) 4.04% CBE/CB (3) 2002 POP POS SOS POP POS SOS 20.35 46.18 33.48 20.42 46.08 33.50 0.07 0.4 0.21 0.21 1.1 0.60 0.05 0.1 0.15 0.07 0.1 0.18 0.07 0.2 0.21 0.21 0.6 0.60 0.12 0.6 0.32 0.16 0.8 0.44 0.10 0.2 0.29 0.15 0.3 0.41 0.13 0.4 0.38 0.20 0.6 0.55 4.00% CBE/CB (4) POP 12 20.76 0.11 0.5 0.31 0.16 0.8 0.46 POS 12 46.10 0.08 0.2 0.22 0.13 0.3 0.35 SOS 12 33.14 0.13 0.4 0.35 0.23 0.7 0.63
(1) CB from Grenada mixed with CBE type PMF/(Shea + Illip) [35/65] (2) CB from Ghana mixed with CBE type PMF/Shea [50/50] (3) CB from Ivory Coast mixed with CBE type PMF/Sal/Mango [50/25/25] (4) CB from Ivory Coast mixed with CBE type PMF/Shea/Illip [50/25/25]