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APPENDIX IV. REPORT OF THE AD HOC WORKING GROUP ON METHODS OF ANALYSIS

INTRODUCTION

The draft Standard for Sugars (see ALINORM 99/25) had been circulated for government and other interested parties to comment in 1999. The comments that were received and the revised draft Standard for Sugars collated and circulated to participants at the Seventh Session of the Codex Committee on Sugars (held London, from 9 to 11, February, 2000) as Conference Room Document 2. Amongst the comments were a number on the analytical methodology to be used in the Standard.

An ad hoc Working Group, the membership of which is given below, was convened at the Seventh Session of CCS at which the comments received were reviewed. The ad hoc Working Group made the recommendations given below for the methods of analysis provisions in the draft Sugar Standard.

MEMBERSHIP OF THE AD HOC WORKING GROUP ON METHODS OF ANALYSIS

The following countries and organizations participated in the Working Group: Cameroon, Canada, Germany, Hungary, India, the Philippines, Spain, the United Kingdom, the United States of America, CFFS, ICUMSA, WSRO.

RECOMMENDATIONS OF THE AD HOC WORKING GROUP ON METHODS OF ANALYSIS

The ad hoc Working Group discussed Conference Room Document 2 and other verbal suggestions made during its meetings.

The Working Group was also aware of the Codex requirements for laboratory quality standard requirements for laboratories involved in the import/export of foods.

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GENERAL COMMENT

SUBMITTED COMMENTS

Canada: The proposed revisions include a statement that “ Those countries proposing new methods for inclusion in the Standard for Sugars were invited to send them directly to the CCMAS for consideration for endorsement.” It is Canada’s position that methods must receive approval from the Sugar Committee before they are committed for endorsement by CCMAS. Therefore any new methods must be sent to the Sugars Committee first not CCMAS.

COMMENTS AND CONCLUSIONS OF WORKING GROUP: ACCEPTED BY WORKING GROUP

SECTION 6.1.3: POLARISATION IN POWDERED SUGAR

PRESENT REQUIREMENTS

ICUMSA (1994) GS 2/3-1, after filtration if necessary to remove any anti-caking agent (endorsed as Type II).

SUBMITTED COMMENTS

ICUMSA: With respect to measurement of Polarisation of powdered sugar to which starch has been added ICUMSA agrees to the addition of sentence “Where the anticaking agent is starch, removal by filtration or centrifugation may not be possible. So ICUMSA is developing another method for such agents.”

CEFS: When starch is present, filtration is not always possible. Propose to add a sentence indicating that polarisation is not measurable for a technical reason in powdered sugar containing starch.

COMMENTS AND CONCLUSIONS OF WORKING GROUP

The Working Group accepts comments and suggests that a footnote to the Standard be given: “Care needs to be taken if anti-caking agents such as starch are present as the method may then not be appropriate.” It was noted that the CEFS representative was of the opinion that the determination of powdered sugar containing starch was not always feasible but that the white sugar used to make the powdered sugar should meet the White Sugar Standard.

ACTION:

Maintain: ICUMSA (1994) GS 2/3-1, after filtration if necessary to remove any anti-caking agent. (endorsed as Type II).

Include a footnote: “Care needs to be taken if anti-caking agents such as starch are present as the method may then not be appropriate.”

SECTION 6.8.1 SULFUR DIOXIDE IN WHITE SUGAR, PLANTATION OR MILL WHITE SUGAR, SOFT WHITE SUGAR AND SOFT BROWN SUGAR, POWDERED SUGAR, POWDERED DEXTROSE AND RAW CANE SUGAR

PRESENT REQUIREMENTS

ICUMSA (1998) GS 2/3-35 / NMKL 135 (1990) / EN 1988-2 (1998)

SUBMITTED COMMENTS

ICUMSA requests ICUMSA (1998) GS 2/3-35 be retained. This method is applicable horizontally in foods and also employs safe reagents

COMMENTS AND CONCLUSIONS OF WORKING GROUP

The Indian delegation suggested that ICUMSA method (1994) GS2-33 (rosaniline procedure) be also permitted as an alternative Type III method. This was accepted by the Working Group. However it was noted that this method employed potentially carcinogenic reagents and so should be used with care.

ACTION: Replace by

ICUMSA (1998) GS 2/3-35 / NMKL 135 (1990) / EN 1988-2 (1998) (Type II method) and

ICUMSA method (1994) GS2-33 (Type III method).

SECTION 6.10: ARSENIC

PRESENT REQUIREMENTS

AOAC 952.13 (Codex general method) or ICUMSA (1994) GS 2/3 - 25.

SUBMITTED COMMENTS

ICUMSA requests that in addition to methods listed suggest addition of ICUMSA (1994) GS2/3-23 (which is to become method ICUMSA (2000) GS2/3 - 23 in 2000.)

COMMENTS AND CONCLUSIONS OF WORKING GROUP

The Working Group accepted the ICUMSA request. It noted that the AOAC INTERNATIONAL method may be dated but that in future it was probable that for trace elements a performance based approach would be adopted by the Codex Alimentarius Commission (currently under discussion in CCMAS).

ACTION: Replace by

AOAC 952.13 (Codex general method) (Type II method), ICUMSA (1994) GS 2/3 - 25 (Type III method) and ICUMSA (1994) GS2/3-23 (Type III method).

SECTION 6.11 LEAD

PRESENT REQUIREMENT

AOAC 997.15 - graphite furnace AA method (Type II method) or ICUMSA (1998) GS 2/3 - 24 (Type II method - identical to AOAC method).

COMMENTS AND CONCLUSIONS OF WORKING GROUP

The Indian delegation suggested that ICUMSA GS 2/1/3 - 27 (1994) be included as a Type IV method. This was accepted by the Working Group.

ACTION: Replace by

AOAC 997.15 - graphite furnace AA method (Type II method) or ICUMSA (1998) GS 2/3 - 24 (Type II method - identical to AOAC method) and ICUMSA GS 2/1/3 - 27 (1994) (Type IV).

SECTION: ANNEX 2.2: CONDUCTIVITY ASH IN FRUCTOSE

PRESENT METHOD

ICUMSA (1994) GS 2/3 - 17 (Type I)

COMMENTS AND CONCLUSIONS OF WORKING GROUP

The Working Group accepted the CCMAS recommendation that this method replace ICUMSA (1994) GS 1/3/4/7/8 - 13.

ACTION: MAINTAIN

ICUMSA (1994) GS 2/3 - 17 (Type I)

SECTION: ANNEX 3: INVERT SUGAR CONTENT

GENERAL COMMENT

CEFS commented that ICUMSA is currently examining methods of invert sugar determination. It seems that current methods could be abandoned in several years and it will then be necessary to adapt the methods of analysis of the standard for sugars.

COMMENTS AND CONCLUSIONS OF WORKING GROUP

The Working Group noted this and anticipated that the determination of specific sugars (i.e. individually identified sugars, sucrose, fructose etc) would be required in future rather than the determination of “classical sugars” (i.e. total sugars determined by a non-specific procedures, e.g. Luff-Schoorl, Lane and Eynon etc). The development of specific chromatographic methods would be reported on in 2002 at the next Session of ICUMSA.

SECTION: ANNEX 3.1 INVERT SUGAR IN WHITE SUGAR (<0.04% M/M)

PRESENT METHOD

ICUMSA (1997) GS 2/3-5 (Type I).

SUBMITTED COMMENTS

ICUMSA requests that ICUMSA (1997) GS 2/3-5 be retained. This and a proposed titrimetric alternative are to be tested against a new enzymic method during 23rd session of ICUMSA with appropriate Recommendations to be made in 2002.

COMMENTS AND CONCLUSIONS OF WORKING GROUP

The Working Group noted that it would be difficult to include more than one Type I method in the Standard. The decision on which method should be included in the Standard at its next revision should be made in the light of the ICUMSA work to be reported in 2002.

ACTION: Maintain

ICUMSA (1997) GS 2/3-5 (Type I)

SECTION: ANNEX 3.2 INVERT SUGAR IN PLANTATION OR MILL WHITE SUGAR (0.1% M/M)

PRESENT METHOD

ICUMSA (1994) GS 1/3/7 - 3 (Type I method).

COMMENTS AND CONCLUSIONS OF WORKING GROUP

The Indian delegation requested that ICUMSA GS 2-6 1998 (Modified Ofner Method) be given in the Standard because the range of application of the method was more appropriate for the concentrations given in the draft Standard and also was more scientifically sound (the lower limit for GS 1/3/7 - 3 is given as 0.25% by ICUMSA).

However, it was noted that this method had only been tentatively adopted by ICUMSA and is presently being further tested with a view to results being reported in 2002. When tested on sugars with low invert sugar content (0.017%) the method was not satisfactory; when tested on 0.04 to 0.09% levels it was found to be satisfactory. The Modified Ofner method was accepted by the Working Group as being most appropriate. It also noted that both methods cannot be included in the Standard as they are both Type I, empirical, procedures

ACTION: Replace by

ICUMSA GS 2-6 1998 (lType I method).

SECTION: ANNEX 7: COLOUR

GENERAL COMMENT

ICUMSA commented that ICUMSA Method (1998) GS2-10 is supported for application to white sugars only. For PMWS, powdered sugars and soft white sugars ICUMSA requests the retention of method ICUMSA (1994) GS2/3-9.

SECTION: ANNEX 7.1: COLOUR IN WHITE SUGAR, POWDERED SUGAR, PLANTATION OR MILL WHITE SUGAR AND SOFT WHITE SUGAR

PRESENT METHOD

ICUMSA (1994) GS2/3-9 (Type I method)

SUBMITTED COMMENTS

India recommends method ICUMSA (1998) GS2-10 is used for determination of colour in white sugars. See also ICUMSA comments above.

COMMENTS AND CONCLUSIONS OF WORKING GROUP

There was extensive discussion on this topic. The Working Group noted that the determination of colour in sugars is an empirical procedure (i.e. a Codex Type I method) so only one method may be given in the Standard. The Indian delegation now wished to apply ICUMSA GS 2 - 10 to all sugars listed in 7.1. However, on circulation of the draft Standard in 1999 the ICUMSA method GS 2 - 9 was given (see ALINORM 99/25). In response to that document the Indian delegation had commented on its inapplicability and wished the method to be replaced by ICUMSA (1998) GS2-10 (see CRD 2) for all white sugars whilst ICUMSA requested the replacement for only White Sugar.

Some members of the Working Group were therefore hesitant to recommend replacement of GS 2 - 9 by GS 2 - 10 for other sugars than White Sugar.

This topic had been extensively discussed at the last ICUMSA Session (Berlin, 1998). The recommendations at from that meeting were:

“The scope of Method GS 2/3 - 9 should state explicitly that the method is not applicable to samples other than [ICUMSA] white sugars.

Based on the good experiences with the former ICUMSA Method 4 (before 1978) and the results of the collaborative study of Method GS 2/3 - 10 (1997), this method is adopted as a new Official ICUMSA method GS 2 - 10 (1998)

It should be noted that results of Methods GS 2/3 - 9 and GS 2 - 10 are principally not comparable, and the method used should always be stated with the results.”

The method GS 2 -10 is currently being prepared for publication by ICUMSA; the final text is not yet available.

11 members of the Working Group wished to replace GS 2/3 - 9 by GS 2 - 10 for white sugar, powdered sugar and soft white sugar (i.e. for sugars with < 60 ICUMSA Units).

The majority of the delegates present at the Working Group wished to replace GS 2/3 - 9 by GS 2 - 10 for plantation or white mill sugar.

The Plenary Session should note that this was the only point of contention within the Working Group.

ACTION; Replace by:

Colour in White Sugar, Powdered Sugar and Soft White Sugar

ICUMSA (1998) GS2-10 (unanimous agreement).

Colour in Plantation or Mill White Sugar

ICUMSA (1998) GS2-10 but noting that there was not unanimity on this recommendation.


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