BS ISO 3632-2-2010 Spices Saffron (Crocus sativus L ) Test methods《香料 藏红花(Crocus sativus L ) 试验方法》.pdf

1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS ISO 3632-2:2010Spices Saffron (Crocus sativus L.)Part 2: Test methodsBS ISO 3632-2:2010 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO

2、3632-2:2010. Itsupersedes DD ISO/TS 3632-2:2003 which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee AW/7, Spices and condiments.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purpor

3、t to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. BSI 2010ISBN 978 0 580 62785 9ICS 67.220.10Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards

4、 Policy and Strategy Committee on 31 October 2010.Amendments issued since publicationDate Text affectedBS ISO 3632-2:2010Reference numberISO 3632-2:2010(E)ISO 2010INTERNATIONAL STANDARD ISO3632-2First edition2010-10-01Spices Saffron (Crocus sativus L.) Part 2: Test methods pices Safran (Crocus sativ

5、us L.) Partie 2: Mthodes dessai BS ISO 3632-2:2010ISO 3632-2:2010(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing policy, this file may be printed or viewed but shall not be edited unless the typefaces which are embedded are licensed to and install

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9、 without permission in writing from either ISO at the address below or ISOs member body in the country of the requester. ISO copyright office Case postale 56 CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Published in Switzerland ii ISO 2010 Al

10、l rights reservedBS ISO 3632-2:2010ISO 3632-2:2010(E) ISO 2010 All rights reserved iiiContents Page Foreword iv 1 Scope1 2 Normative references1 3 Terms and definitions .1 4 Tests and sample sizes.2 5 Identification test.4 6 Microscopic examination of saffron5 7 Determination of moisture and volatil

11、e matter content.8 8 Determination of floral waste content of saffron in filaments and cut filaments .10 9 Determination of foreign matter content of saffron in filaments and cut filaments.10 10 Crushing and sieving of the samples for tests described in Clauses 6, 14, 15 and 16 .11 11 Determination

12、of extract soluble in cold water 12 12 Determination of total ash 12 13 Determination of acid-insoluble ash .12 14 Determination of the main characteristics using a UV-vis spectrometric method.12 15 Detection of artificial coloring: identification of synthetic water-soluble acidic colorants Thin-lay

13、er chromatography method14 16 Detection of artificial coloring: identification of synthetic water-soluble acidic colorants High performance liquid chromatography (HPLC) 18 Annex A (informative) Example for the expression of results for a microscopic examination 25 Annex B (informative) Photographic

14、references for microscopic identification27 Annex C (informative) Example of a UV-vis profile of an aqueous extract of saffron .30 Annex D (informative) Examples of chromatograms 31 Bibliography36 BS ISO 3632-2:2010ISO 3632-2:2010(E) iv ISO 2010 All rights reservedForeword ISO (the International Org

15、anization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been establi

16、shed has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardizatio

17、n. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting.

18、Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such pat

19、ent rights. ISO 3632-2 was prepared by Technical Committee ISO/TC 34, Food products, Subcommittee SC 7, Spices, culinary herbs and condiments. This second edition of ISO 3632-2 cancels and replaces ISO/TS 3632-2:2003, which has been technically revised. ISO 3632 consists of the following parts, unde

20、r the general title Spices Saffron (Crocus sativus L.): Part 1: Specification Part 2: Test methods BS ISO 3632-2:2010INTERNATIONAL STANDARD ISO 3632-2:2010(E) ISO 2010 All rights reserved 1Spices Saffron (Crocus sativus L.) Part 2: Test methods 1 Scope This part of ISO 3632 specifies test methods fo

21、r dried saffron obtained from the Crocus sativus L. flower. It is applicable to saffron: a) filaments and cut filaments; b) powder. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies.

22、For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 928, Spices and condiments Determination of total ash ISO 930, Spices and condiments Determination of acid-insoluble ash ISO 941, Spices and condiments Determination of cold water-soluble ex

23、tract ISO 948, Spices and condiments Sampling ISO 3632-1, Spices Saffron (Crocus sativus L.) Part 1: Specification 3 Terms and definitions For the purposes of this document, the terms and definitions given in ISO 3632-1 and the following apply. 3.1 moisture and volatile matter content loss of mass f

24、raction determined under the conditions specified in this part of ISO 3632 NOTE Moisture and volatile matter content is expressed as a percentage mass fraction of the sample. BS ISO 3632-2:2010ISO 3632-2:2010(E) 2 ISO 2010 All rights reserved3.2 colouring strength 1%1cmA , 440 nm absorbance at the m

25、aximum wavelength (about 440 nm) of crocins for a 1 g/100 ml solution of test sample using a 1 cm quartz cell NOTE Colouring strength is mainly due to the content of crocins. 3.3 UV-vis profile of saffron extract spectrum obtained between 200 nm and 700 nm NOTE An example is given for information in

26、 Figure C.1. 3.4 limit of detection LOD minimum amount or concentration of the analyte in a test sample which can be detected reliably, but not necessarily quantified, as demonstrated by a collaborative trial or other appropriate validation 3.5 minimum required performance limit MRPL minimum content

27、 of an analyte in a sample, which at least has to be detected and confirmed 4 Tests and sample sizes 4.1 Minimum mass of the laboratory sample Sampling methods for spices and condiments are specified in ISO 948. Considering the high cost of saffron, the mass of sample received in the laboratories fo

28、r carrying out the tests is often limited. The minimum mass of the laboratory sample shall be 23 g (11,5 g 2) for saffron filaments and cut filaments and 13,5 g (6,75 g 2) for saffron powder in order to carry out the standard analyses in duplicate. It is recommended that larger quantities of sample

29、be placed at the disposal of the laboratories in case of dispute. Since the mass of the test portion is low, it is advisable that it be taken from a homogenized sample. 4.2 Tests required and test sample sizes See Table 1 for saffron in filaments, cut filaments and Table 2 for saffron in powder. BS

30、ISO 3632-2:2010ISO 3632-2:2010(E) ISO 2010 All rights reserved 3Table 1 Saffron in filaments and cut filaments forms Analysis step Procedure (laboratory sample: 11,5 g 2 = 23 g)Test sample g Comments Corresponding clause 1 Identification test 5 New test sample Non-destructive test 5 2 Microscopic ex

31、amination 0,05 Test sample from step 1 6 3 Determination of floral waste content 3 Test sample from step 1 Non-destructive test 8 4 Determination of foreign matter 3 Test sample from step 3 Test sample is reconstituted after reincorporating floral waste 9 5 Determination of extract soluble in cold w

32、ater 2 Test sample from step 4 11 6 Determination of moisture and volatile matter content 2,5 New test sample Keep the test sample for determination of total ash and acid-insoluble ash 7 7 Determination of total ash 2 Remains of the test sample from step 6 12 8 Determination of acid-insoluble ash Te

33、st sample produced after step 7 13 9 Crushing and sieving 4 New test sample Carry out the sieving in accordance with Clause 10 to obtain a powder of which 95 % mass fraction passes through a 500 m sieve. Reincorporate whatever remains on the sieve in the receptacle of the sieve 10 10 Determination o

34、f main characteristics 0,5 Test sample from step 9, after sieving 14 11 Thin-layer chromatography (TLC): identification of artificial colorants 0,5 Test sample from step 9, before sieving HPLC (step 12) may alternatively or additionally be performed. In the latter case, use the extract for both meth

35、ods 15 12 High performance liquid chromatography (HPLC): identification of artificial colorants 0,5 Test sample from step 9, before sieving TLC (step 11) may alternatively or additionally be performed. In the latter case, use the extract for both methods 16 NOTE There remain 4,50 g laboratory sample

36、 which can be used for further tests or to repeat certain analyses if necessary. BS ISO 3632-2:2010ISO 3632-2:2010(E) 4 ISO 2010 All rights reservedTable 2 Saffron in powder form Analysis step Procedure (laboratory sample: 6,75 g 2 = 13,5 g) Test sampleg Comments Corresponding clause 1 Identificatio

37、n test 0,2 New test sample Do not continue with the analysis if the colorimetric analysis is not correct 5 2 Microscopic examination 0,05 New test sample 6 3 Determination of moisture and volatile matter content 2,5 New test sample Keep the test sample for determination of total ash and acid-insolub

38、le ash 7 4 Determination of total ash 2 Remains of the test sample from step 3 12 5 Determination of acid-insoluble ash Remains of the test sample from step 4 13 6 Crushing and sieving 4 New test sample Verify that 95 % mass fraction of the powder passes through a 500 m sieve. Reincorporate whatever

39、 remains on the sieve in the receptacle of the sieve 10 7 Determination of extract soluble in cold water 2 Test sample from step 6 11 8 Determination of main characteristics 0,5 Test sample from step 6, after sieving 14 9 Thin-layer chromatography (TLC): identification of artificial colorants 0,5 Te

40、st sample from step 6, before sieving HPLC (10) may alternatively or additionally be performed. In the latter case, use the extract for both methods 15 10 High performance liquid chromatography (HPLC): identification of artificial colorants 0,5 Test sample from step 6, before sieving TLC (9) may alt

41、ernatively or additionally be performed. In the latter case, use the extract for both methods 16 NOTE There remain 1 g laboratory sample which can be used for further tests or to repeat certain analyses if necessary. 5 Identification test 5.1 General This preliminary test may make the subsequent ana

42、lyses unnecessary if it shows that the saffron is not pure. 5.2 Saffron in filaments and cut filaments 5.2.1 Principle The saffron is examined visually with a magnifying glass. 5.2.2 Apparatus 5.2.2.1 Magnifying glass, with a magnification of 10 times max. 5.2.2.2 Watch glass, of suitable size. BS I

43、SO 3632-2:2010ISO 3632-2:2010(E) ISO 2010 All rights reserved 55.2.3 Procedure Spread out the test sample of saffron in filaments and cut filaments (Table 1) on the watch glass (5.2.2.2) and examine it with the magnifying glass (5.2.2.1). 5.2.4 Interpretation of results All the filaments shall belon

44、g to the plant Crocus sativus L. Reject the sample if vegetable matter other than that belonging to Crocus sativus L. is found. 5.3 Saffron in powder form 5.3.1 Principle A colorimetric reaction is used. 5.3.2 Reagents During the analysis, unless otherwise stated, use only reagents of recognized ana

45、lytical grade and distilled or demineralized water or water of equivalent quality. 5.3.2.1 Sulfuric acid, mass concentration 1,19 g/l. 5.3.2.2 Diphenylamine solution. Add 0,1 g diphenylamine to 20 ml sulfuric acid (5.3.2.1) and 4 ml water. The diphenylamine shall not produce any coloured reaction wi

46、th the sulfuric acid. 5.3.3 Porcelain dish, with flat bottom. 5.3.4 Procedure Use the 0,2 g test sample of saffron (see Table 2) as test portion. Gradually add the test portion to the porcelain dish (5.3.3) containing the diphenylamine solution (5.3.2.2). 5.3.5 Interpretation of results Pure saffron

47、 immediately produces a blue colour, which rapidly turns reddish brown. In the presence of nitrates, the blue colour persists. 6 Microscopic examination of saffron 6.1 General The method is applicable to the examination of saffron in powder, filaments, and cut filament forms in order to determine wh

48、ether the sample consists exclusively of stigmas belonging to Crocus sativus L. and to highlight any floral waste and foreign matter. 6.2 Principle The identity of saffron in powder and crushed filament form is verified. Foreign matter and floral waste, if any, are identified by the observation of a

49、natomical elements by using microscopy under the conditions described in 6.5. The percentages relating to the observed elements may be determined if required (see Annexes A and B). BS ISO 3632-2:2010ISO 3632-2:2010(E) 6 ISO 2010 All rights reserved6.3 Reagents During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and distilled or demineralized water or water of equivalent purity. 6.3.1 Iodine in iodide solution, aqueous solution of iodine in potassium