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1、DRAFT FOR DEVELOPMENT DD CEN/TS 13130-16:2005 Materials and articles in contact with foodstuffs Plastics substances subject to limitation Part 16: Determination of caprolactam and caprolactam salt in food simulants ICS 67.250 DD CEN/TS 13130-16:2005 This Draft for Development was published under the
2、 authority of the Standards Policy and Strategy Committee on 16 September 2005 BSI 16 September 2005 ISBN 0 580 46071 1 National foreword This Draft for Development is the official English language version of CEN/TS 13130-10:2005. This publication is not to be regarded as a British Standard. It is b
3、eing issued in the Draft for Development series of publications and is of a provisional nature because the method was not evaluated using recognized ring trial procedures. As a consequence there are no reproducibility data for the method. It should be applied on this provisional basis, so that infor
4、mation and experience of its practical application may be obtained. Comments arising from the use of this Draft for Development are requested so that UK experience can be reported to the European organization responsible for its conversion to a European standard. A review of this publication will be
5、 initiated 2 years after its publication by the European organization so that a decision can be taken on its status at the end of its 3-year life. Notification of the start of the review period will be made in an announcement in the appropriate issue of Update Standards. According to the replies rec
6、eived by the end of the review period, the responsible BSI Committee will decide whether to support the conversion into a European Standard, to extend the life of the Technical Specification or to withdraw it. Comments should be sent in writing to the Secretary of BSI Subcommittee CW/47/1 Migration
7、from plastics, at British Standards House, 389 Chiswick High Road, London W4 4AL, giving the document reference and clause number and proposing, where possible, an appropriate revision of the text. A list of organizations represented on this subcommittee can be obtained on request to its secretary.
8、Cross-references The British Standards which implement international or European publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or
9、 of British Standards Online. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Summary of pages This document comprises a front cover, an inside front cover, the CEN/TS title page, pages 2 to 16, an inside bac
10、k cover and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. DateComments W - - - - - - - - - - 7 - - 7- - - - - 7- - - - - 7 - - - - - - - - 98 % (GC). 4.1.2 Aza-2-cyclononanone, (8-aminooctan
11、oic acid lactam; 8-Caprylolactam), C8H15NO molecular weight 141,2, purity 99 %. 4.2 Chemicals 4.2.1 Ethanol, absolute 4.2.2 n-Heptane 4.2.3 Methanol 4.2.4 Water, deionized 4.3 Solutions 4.3.1 Ethanol/water = 1:2 Measure 200 ml ethanol (4.2.1) and make up with water (4.2.4) to 600 ml. 4.3.2 Standard
12、stock solution of caprolactam in methanol (0,5 mg/ml) Weigh to the nearest 0,1 mg approximately 50 mg of caprolactam (4.1.1) into a 100 ml volumetric flask. Dissolve the caprolactam in methanol and make up to the mark with methanol (4.2.3). Calculate the exact concentration in milligrams of caprolac
13、tam per millilitre solution. Repeat the procedure to obtain a second stock solution. NOTE The solution can be stored in a well-closed container in the dark for a maximum period of 3 months at any temperature between - 20 C to + 20 C. 4.3.3 Internal standard stock solution of caprylolactam in methano
14、l (0,35 mg/ml) Weigh to the nearest 0,1 mg approximately 70 mg of caprylolactam (4.1.2) into a 200 ml volumetric flask. Dissolve the caprylolactam in methanol and make up to the mark with methanol (4.2.3). Calculate the exact concentration in milligrams caprylolactam per millilitre of solution. NOTE
15、 The solution can be stored in a well-closed container in the dark for a maximum period of 3 months at any temperature between - 20 C and + 20 C. 4.3.4 Diluted internal standard solution of caprylolactam in methanol (0,07 mg/ml) Transfer by pipette 10,0 ml of the internal standard stock solution (4.
16、3.3) into a 50 ml volumetric flask and make up to the mark with methanol (4.2.3). Calculate the concentration in milligrams of caprylolactam per millilitre of solution. DD CEN/TS 13130-16:2005 8 4.3.5 Standard solutions Add to a series of 25 ml volumetric flasks, 0 ml, 1 ml, 2 ml, 4 ml, 6 ml and 8 m
17、l of the standard stock solution of caprolactam (4.3.2). Add to each of the flasks 5,0 ml of the internal standard stock solution of caprylolactam (4.3.3) and make up to the mark with methanol (4.2.3). The standards thus obtained contain approximately 0 g/ml, 20 g/ml, 40 g/ml, 80 g/ml, 120 g/ml and
18、160 g/ml of caprolactam and 70 g of caprylolactam per millilitre of methanol. Calculate the exact concentrations in micrograms per millilitre of methanol. Repeat the procedure using the second standard stock solution to obtain a second series of standard solutions. 5 Apparatus NOTE An instrument or
19、item of apparatus is listed only where it is special or made to a particular specification, usual laboratory glassware and equipment being assumed to be available. 5.1 Gas chromatograph, equipped with a flame ionization detector and preferably with an automatic injection sampler, capable of separati
20、ng caprolactam fully from caprylolactam as well as from peaks originating from simulants and/or solvents used. Appropriate operating conditions shall be established for the specific equipment used for the determination. NOTE 1 The following chromatographic columns and conditions have been found to b
21、e satisfactory: Column 1 25 m x 0,32 mm fused silica WCOT provided with a 1,2 m thick layer of 7 % cyanopropyl, 7 % phenyl, 85 % methyl and 1 % vinylpolysiloxane. DD CEN/TS 13130-16:2005 9 GC parameters: Column oven 200 C Injector 240 C Detector 250 C Carrier gas helium Inlet pressure 150 kPa Flow 3
22、 ml/min Injector split (split ratio 1:14) Injection volume: 0.5 l FID gasses optimized according to the manufacturers specifications. GC apparatus should be optimized according to manufacturers instruction. Occasionally, double peaks for caprolactam have been observed. Reasons for this phenomenon sh
23、ould be found in the injection system. Cleaning or exchange of the injector liner is recommended to overcome the problem. In any case, double peaks should not be evaluated. NOTE 2 Other columns that have been found to be suitable are as follows: Column 2 50 m x 0,2 mm fused silica coated with 0,5 m
24、methylsilicone. Temperature programme 2 min at 80 C then ramped at 5 C per minute to 230 C Carrier gas helium at 220,6 kPa Injection temperature 250 C Detector temperature 280 C Column 3 2 m x 2 mm stainless steel column, packed with Gaschrom Q 100 mesh to 120 mesh coated with 10 % of polyethylenegl
25、ycolterephthalate (SP 1000). Temperature 210 C, isothermal Carrier gas nitrogen 25 ml per minute Injection temperature 260 C Detector temperature 260 C 5.2 Mechanical shaker (reciprocal motion) 6 Samples 6.1 General Laboratory samples of the food simulant to be analyzed shall be obtained as describe
26、d in EN 13130-1. Samples shall be kept refrigerated with the exclusion of light. Analyte-free samples of relevant food simulants of the same type as those to be analyzed shall also be prepared for use for calibration purposes. 6.2 Test sample preparation 6.2.1 Aqueous solutions Pipette 1,0 ml of the
27、 diluted internal standard solution (4.3.4) into a conical flask, add 4,0 ml of food simulant obtained from the migration experiment (see EN 13130-1) and mix thoroughly. Transfer a small amount of the solution into a vial suitable for GC injections. DD CEN/TS 13130-16:2005 10 6.2.2 Olive oil Weigh 1
28、5 g 0,1 g of olive oil obtained from the migration experiment (see EN 13130-1) into a 50 ml conical flask. Add 2,0 ml of diluted internal standard solution (4.3.4) and mix. Add 15 ml 1 ml n-heptane (4.2.2), mix and add 8,0 ml of ethanol/water = 1:2 (4.3.1) using a volumetric pipette. Gently shake fo
29、r 10 min using a mechanical shaker (5.2). Allow the phases to separate for approximately 30 min. Retract by means of a pipette approximately 5 ml of the aqueous (lower) layer and pass the solution, to retain any oil, through a small glass funnel provided with a small plug of cotton wool, into a vial
30、 suitable for GC injections. NOTE Alternatively, the mixture can be put in a separating funnel and shaken by hand for 1,5 min. 6.3 Blank sample preparation Treat food simulants that have not been in contact with packaging material in the same way as described in Clause 6.2. 6.4 Calibration sample pr
31、eparation 6.4.1 Calibration samples for aqueous food simulants Pipette into a series of conical flasks 1,0 ml of each of the standard solutions (4.3.5) and 4,0 ml of analyte free food simulant, water, 3 % w/v aqueous acetic acid or 15 % v/v aqueous ethanol, and mix thoroughly. The solutions thus obt
32、ained contain approximately 0 g/ml, 5 g/ml, 10 g/ml, 20 g/ml, 30 g/ml or 40 g of caprolactam and 17,5 g of caprylolactam per millilitre of food simulant. 6.4.2 Calibration samples for olive oil Weigh into a series of 50 ml conical flasks 15 g 0,1 g of analyte free olive oil. Add, to each flask, 2,0
33、ml of the standard solutions (4.3.5) and mix. The mixtures thus obtained contain approximately 0 g/g, 2,7 g/g, 5,3 g/g, 10,7 g/g, 16,0 g/g or 21,3 g of caprolactam and 9,3 g of caprylolactam per gram of olive oil. Extract each olive oil calibration sample as follows. Add 15 ml 1 ml n-heptane (4.2.2)
34、, mix and add 8,0 ml of ethanol/water = 1:2 (3.3.1) using a volumetric pipette. Gently shake for 10 min using a mechanical shaker (5.2). Allow the phases to separate for approximately 30 min. Retract by means of a pipette approximately 5 ml of the aqueous (lower) layer and pass the solution through
35、a small glass funnel, provided with a small plug of cotton wool to retain any olive oil, into a vial suitable for GC injections. NOTE Alternatively, the mixture can be placed in a separating funnel and shaken by hand for 1,5 min. 7 Procedure 7.1 GC analysis The test samples, blanks and calibration s
36、amples prepared in 6.1 to 6.3 shall be analyzed as they are without any further sample treatment. Each solution shall be injected at least in duplicate. Examine the baseline stability and response linearity of the detector when starting GC headspace measurements. DD CEN/TS 13130-16:2005 11 NOTE 1 Th
37、e detector should be able to detect at least 40 pg on column of caprolactam at a signal to noise ratio of 3:1. Maintain the same headspace GC operating conditions throughout the measurement of all samples and calibration solutions. NOTE 2 Under the conditions given in 5.2 the retention time was 3,0
38、min and 5,0 min for caprolactam and caprylolactam, respectively. 7.2 Calibration Inject each of the working standard solutions as prepared in 6.4.1 and 6.4.2, in duplicate, into the GC column. Measure the peak height or area of caprolactam and caprylolactam. Divide the caprolactam peak height/area b
39、y the caprylolactam peak height/area and graphically plot peak ratios (PR) against the concentration of caprolactam in the calibration samples in milligrams per kilogram assuming a density of 1,0g per millilitre of food simulant. NOTE Commission Directive 90/128/EEC 1 states that the specific gravit
40、y of all simulants should conventionally be assumed to be 1. Milligrams of substance released per litre of simulant will thus correspond numerically to milligrams of substance released per kilogram of simulant and, taking into account of the provisions laid down in Directive 82/711/EEC 3, to milligr
41、ams of substance released per kilogram of foodstuff. The calibration graph shall be rectilinear and the correlation coefficient shall be 0,996 or better. The two sets of calibrant solutions made from independently prepared stock solutions shall be cross- checked by generating two calibration curves,
42、 which on the basis of peak ratio measurement, shall agree to within 5 % of one another. 7.3 Evaluation of data NOTE The following calculations assume that for all measurements exactly the same mass or volume of water, 3 % acetic acid, 15 % ethanol or olive oil has been used and, for the internal st
43、andard, that invariably the same volume of internal standard solution has been added. 7.3.1 GC interferences If the GC chromatogram of the blank sample (7.2) shows an interfering peak in the caprolactam region, use different chromatographic conditions and/or use alternative food simulants, e.g. sunf
44、lower oil or a mixture of synthetic triglycerides, instead of olive oil. NOTE No interferences arising from the four conventional EU food simulants, have so far been observed using the method. 7.3.2 Calculation of analyte level 7.3.2.1 Graphical determination Calculate the average of peak area/heigh
45、t ratio (PR) values obtained from the test samples according to 7.1 and read the caprolactam concentration of the test samples from the calibration graph (7.2). 7.3.2.2 Calculation from the regression parameters If the regression line equation is: bxaPRy DD CEN/TS 13130-16:2005 12 where yPR is the p
46、eak height/area ratio of caprolactam/ caprylolactam; a is the slope of the regression line; x is the concentration of caprolactam in the food simulant in milligrams per kilogram; b is the intercept of the regression line, then the concentration of caprolactam is given by: a by C fsCap, where CCap,fs
47、 is the concentration of caprolactam in milligrams per kilogram. Both procedures yield directly the caprolactam concentration in the food simulant in milligrams per kilogram. The method applying calculation from the regression parameters is the preferred method. 7.3.3 Calculation of the specific mig
48、ration of caprolactam Depending on the fill volume of the test material and on the surface area/food simulant, the caprolactam concentration in the test sample as determined according to 7.3.2 may need mathematical transformation to calculate the specific migration value to be compared with the specific migration limit (SML). For guidanc