ANALYTICAL METHODS FOR FOOD ADDITIVES
E110: SUNSET YELLOW INTRODUCTION METHODS OF ANALYSIS RECOMMENDATIONS REFERENCES APPENDIX: METHOD PROCEDURE SUMMARIES SUMMARY OF METHODS FOR SUNSET YELLOW IN FOODS SUMMARY OF STATISTICAL PARAMETERS FOR SUNSET YELLOW IN FOODS PERFORMANCE CHARACTERISTICS FOR SUNSET YELLOW IN LEMONADE (PRE-TRIAL SAMPLES) PERFORMANCE CHARACTERISTICS FOR SUNSET YELLOW IN BITTER SAMPLES E122: AZORUBINE (CARMOISINE) SUMMARY OF METHODS FOR AZORUBINE IN FOODS SUMMARY OF STATISTICAL PARAMETERS FOR AZORUBINE IN FOODS PERFORMANCE CHARACTERISTICS FOR AZORUBINE IN COLLABORATIVE TRIAL SAMPLES PERFORMANCE CHARACTERISTICS FOR AZORUBINE IN BITTER SAMPLES CONTENTS E141: COPPER COMPLEXES OF CHLOROPHYLLS AND CHLOROPHYLLINS SUMMARY OF METHODS FOR CU COMPLEXES OF CHLOROPHYLLS AND CHLOROPHYLLINS IN FOODS SUMMARY OF STATISTICAL PARAMETERS FOR CU COMPLEXES OF CHLOROPHYLLS AND CHLOROPHYLLINS IN FOODS E150C: CARAMEL CLASS III SUMMARY OF METHODS FOR CARAMEL (CLASS III) E160B: ANNATTO EXTRACTS SUMMARY OF METHODS FOR ANNATTO EXTRACTS IN FOODS SUMMARY OF STATISTICAL PARAMETERS FOR ANNATTO EXTRACTS IN FOODS E200–3: SORBIC ACID AND ITS SALTS SUMMARY OF METHODS FOR SORBIC ACID IN FOODS SUMMARY OF STATISTICAL PARAMETERS FOR SORBIC ACID IN FOODS PERFORMANCE CHARACTERISTICS FOR SORBIC ACID IN ALMOND PASTE, FISH HOMOGENATE AND APPLE JUICE PERFORMANCE CHARACTERISTICS FOR SORBIC ACID IN ORANGE SQUASH, COLA DRINKS, BEETROOT, PIE FILLING AND SALAD CREAM E210–13: BENZOIC ACID SUMMARY OF METHODS FOR BENZOIC ACID IN FOODS SUMMARY OF STATISTICAL PARAMETERS FOR BENZOIC ACID IN FOODS PERFORMANCE CHARACTERISTICS FOR BENZOIC ACID IN ALMOND PASTE, FISH HOMOGENATE AND APPLE JUICE PERFORMANCE CHARACTERISTICS FOR BENZOIC ACID IN ORANGE JUICE PERFORMANCE CHARACTERISTICS FOR BENZOIC ACID IN ORANGE SQUASH, COLA DRINKS, BEETROOT AND PIE FILLING E220–8: SULPHITES SUMMARY OF METHODS FOR SULPHITES IN FOODS SUMMARY OF STATISTICAL PARAMETERS FOR SULPHITES IN FOODS PERFORMANCE CHARACTERISTICS FOR SULPHITES IN HOMINY, FRUIT JUICE AND SEAFOOD PERFORMANCE CHARACTERISTICS FOR SULPHITES IN WINE, DRIED APPLES, LEMON JUICE, POTATO FLAKES, SULTANAS AND BEER PERFORMANCE CHARACTERISTICS FOR TOTAL SULPHITE IN SHRIMP, ORANGE JUICE, DRIED APRICOTS, DEHYDRATED POTATO FLAKES AND PEAS PERFORMANCE CHARACTERISTICS FOR TOTAL SULPHITE IN STARCH, LEMON JUICE, WINE COOLER, DEHYDRATED SEAFOOD AND INSTANT MASHED POTATOES PERFORMANCE CHARACTERISTICS FOR TOTAL SULPHITE IN SHRIMP, POTATOES, PINEAPPLE AND WINE PERFORMANCE CHARACTERISTICS FOR FREE SULPHITE IN WINE E249–50: NITRITES APPENDIX 1: METHOD PROCEDURE SUMMARIES (MEAT – DD ENV 12014) APPENDIX 2: METHOD PROCEDURE SUMMARIES (MILK AND MILK PRODUCTS – BS EN ISO 14673) SUMMARY OF METHODS FOR NITRITES IN FOODS SUMMARY OF STATISTICAL PARAMETERS FOR NITRITES IN FOODS PERFORMANCE CHARACTERISTICS FOR NITRITE IN MEAT PRODUCTS PERFORMANCE CHARACTERISTICS FOR NITRITE IN FOODS 10 E297: FUMARIC ACID AND ITS SALTS SUMMARY OF METHODS FOR FUMARIC ACID IN FOODS SUMMARY OF STATISTICAL PARAMETERS FOR FUMARIC ACID IN FOODS PERFORMANCE CHARACTERISTICS FOR FUMARIC ACID IN LAGER BEERS 11 E310–12: GALLATES SUMMARY OF METHODS FOR GALLATES IN FOODS SUMMARY OF STATISTICAL PARAMETERS FOR GALLATES IN FOODS PERFORMANCE CHARACTERISTICS FOR GALLATES IN OILS, LARD AND BUTTER OIL 12 E320: BHA SUMMARY OF METHODS FOR BHA IN FOODS SUMMARY OF STATISTICAL PARAMETERS FOR BHA IN FOODS PERFORMANCE CHARACTERISTICS FOR BHA IN OILS, LARD AND BUTTER OIL 13 E334–7, E354: L-TARTARIC ACID AND ITS SALTS SUMMARY OF METHODS FOR L-TARTARIC ACID IN FOODS SUMMARY OF STATISTICAL PARAMETERS FOR L-TARTARIC ACID IN FOODS PERFORMANCE CHARACTERISTICS FOR L-TARTARIC ACID IN GRAPE JUICES 14 E355–7, E359: ADIPIC ACID AND ITS SALTS APPENDIX 1: METHOD PROCEDURE SUMMARIES (ANALYSIS OF ORANGE DRINKS) APPENDIX 2: METHOD PROCEDURE SUMMARIES: ANALYSIS OF STARCH SUMMARY OF METHODS FOR ADIPIC ACID IN FOODS SUMMARY OF STATISTICAL PARAMETERS FOR ADIPIC ACID IN FOODS PERFORMANCE CHARACTERISTICS FOR ADIPIC ACID IN ORANGE DRINK SAMPLES PERFORMANCE CHARACTERISTICS FOR ADIPIC ACID IN ACETYLATED ADIPYL CROSS-LINKED STARCHES 15 E405, E477: PROPYLENE GLYCOL (PROPAN-1,2-DIOL) SUMMARY OF METHODS FOR PROPYLENE GLYCOL IN FOODS SUMMARY OF STATISTICAL PARAMETERS FOR PROPYLENE GLYCOL IN FOODS 16 E416: KARAYA GUM SUMMARY OF METHODS FOR KARAYA GUM 17 E432–6: POLYSORBATES SUMMARY OF METHODS FOR POLYSORBATES IN FOODS SUMMARY OF STATISTICAL PARAMETERS FOR POLYSORBATES IN FOODS 18 E442: AMMONIUM PHOSPHATIDES SUMMARY OF METHODS FOR PHOSPHORUS IN FOODS SUMMARY OF STATISTICAL PARAMETERS FOR PHOSPHORUS IN FOODS PERFORMANCE CHARACTERISTICS FOR TOTAL PHOSPHORUS IN COLLABORATIVE TRIAL SAMPLES 19 E444: SUCROSE ACETATE ISOBUTYRATE APPENDIX: METHOD PROCEDURE SUMMARY SUMMARY OF METHODS FOR SUCROSE ACETATE ISOBUTYRATE IN FOODS SUMMARY OF STATISTICAL PARAMETERS FOR SUCROSE ACETATE ISOBUTYRATE IN FOODS 20 E472E: MONO/DIACETYL TARTARIC ACID ESTERS OF MONO/DIGLYCERIDES OF FATTY ACIDS SUMMARY OF METHODS FOR MONO/DIACETYL TARTARIC ACID ESTERS OF MONO/DIGLYCERIDES OF FATTY ACIDS IN FOODS SUMMARY OF STATISTICAL PARAMETERS FOR MONO/ DIACETYL TARTARIC ACID ESTERS OF MONO/DIGLYCERIDES OF FATTY ACIDS IN FOODS 21 E476: POLYGLYCEROL ESTERS OF POLYCONDENSED FATTY ACIDS OF CASTOR OIL SUMMARY OF METHODS FOR POLYGLYCEROL POLYRICINOLEATE IN FOODS 22 E481–2: STEAROYL LACTYLATES SUMMARY OF METHODS FOR STEAROYL LACTYLATES IN FOODS SUMMARY OF STATISTICAL PARAMETERS FOR STEAROYL LACTYLATES IN FOODS 23 E483: STEARYL TARTRATE 24 E491–2, E493–4, E495: SORBITAN ESTERS SUMMARY OF METHODS FOR SORBITAN ESTERS IN FOODS SUMMARY OF STATISTICAL PARAMETERS FOR SORBITAN ESTERS IN FOODS 25 E520–3, E541, E554–9, E573: ALUMINIUM SUMMARY OF METHODS FOR ALUMINIUM IN FOODS SUMMARY OF STATISTICAL PARAMETERS FOR ALUMINIUM IN FOODS PERFORMANCE CHARACTERISTICS FOR ALUMINIUM IN MILK POWDER SUMMARY OF KEY STEPS OF PROCEDURES USED IN IUPAC SAMPLE SURVEY 26 E954: SACCHARIN SUMMARY OF METHODS FOR SACCHARIN IN FOODS SUMMARY OF STATISTICAL PARAMETERS FOR SACCHARIN IN FOODS PERFORMANCE CHARACTERISTICS FOR SACCHARIN IN SWEETENER TABLETS PERFORMANCE CHARACTERISTICS FOR SACCHARIN IN LIQUID SWEETENER PERFORMANCE CHARACTERISTICS FOR SODIUM SACCHARIN IN MARZIPAN, YOGURT, ORANGE JUICE, CREAM, COLA AND JAM PERFORMANCE CHARACTERISTICS FOR SODIUM SACCHARIN IN JUICE, SOFT DRINK AND SWEETS PERFORMANCE CHARACTERISTICS FOR SODIUM SACCHARIN IN JUICE, SOFT DRINK AND DESSERT PRELIMINARY TREATMENT OF THE FOOD EXTRACTION AND PURIFICATION OF THE DYE FROM THE PREPARED SOLUTION OR EXTRACT OF THE FOOD SEPARATION OF MIXED COLOURS IF MORE THAN ONE IS PRESENT IDENTIFICATION OF THE SEPARATED DYES THERE ARE NUMEROUS METHODS PUBLISHED FOR THE DETERMINATION OF SUNSET YELLOW IN FOODSTUFFS THE MAJORITY OF THESE METHODS ARE FOR THE DETERMINATION OF VARIOUS WATER-SOLUBLE DYES, INCLUDING SUNSET YELLOW, IN FOODSTUFFS THE EARLY WORKERS ON THE DEVELOPMENT OF METHODS FOR FOOD COLOURS USED PAPER CHROMATOGRAPHY AND TLC BUT OVER THE LAST 20 YEARS HPLC,2–8 SPECTROPHOTOMETRIC,9–15,22 VOLTAMMETRIC20,21 AND MORE RECENTLY CAPILLARY ZONE ELECTROPHORESIS16–19 METHODS HAVE BEEN DEVELOPED AND A SUMMARY OF THESE IS GIVEN IN TABLE 1 1, TOGETHER WITH THE MATRICES TO WHICH THE METHODS APPLY IF STATISTICAL PARAMETERS FOR THESE METHODS ARE AVAILABLE THEY ARE REFERENCES 1 PEARSON’S COMPOSITION AND ANALYSIS OF FOODS, 9 ED KIRK R AND SAWYER R, LONGMAN SCIENTIFIC, HARLOW, (1989) 2 ‘DETERMINATION OF SYNTHETIC COAL-TAR DYES IN SOFT DRINKS, SKIMMED MILKS AND CAKES: COLLABORATIVE TRIAL’, DENNIS J, CHAPMAN S, BRERETON P, TURNBULL J, WOOD R J ASSOC PUBL ANALYSTS (1997) 33, 161–202 3 ‘A REVERSE PHASE HPLC METHOD TO DETERMINE SIX FOOD DYES USING BUFFERED MOBILE PHASE’, BERZASNEVADO J J, GUIBERTEAUCABANILLAS C AND CONTENTOSALCEDO A M ANALYTICAL LETTERS (1998) 31(14), 2513–2535 4 ‘SIMULTANEOUS DETERMINATION OF PRESERVATIVES, SWEETENERS AND COLOURINGS IN SOFT DRINKS BY ION-PAIR REVERSED PHASE HPLC’, ZHOU S, LI J SEPU (1990) 8(1), 54–56 [CHINESE] 5 ‘RAPID DETERMINATION OF PRESERVATIVES, SWEETENERS, FOOD COLOURINGS AND CAFFEINE BY HPLC’, REN Y, GAO Z, HUANG B SHIPIN YU FAJIAO GONGYE (1990) 1, 72–75 [CHINESE] 6 ‘SIMULTANEOUS DETERMINATION OF NINE FOOD ADDITIVES IN BEVERAGES BY HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY (HPLC)’, WU F, ZHANG P SEPU (1992) 10(5), 311–312 [CHINESE] 7 ‘DETERMINATION OF EIGHT SYNTHETIC FOOD COLORANTS IN DRINKS BY HIGH-PERFORMANCE ION E110: SUNSET YELLOW CHROMATOGRAPHY’, CHEN Q C, MOU S F, HOU X P, RIVIELLO J M, NI Z M JOURNAL OF CHROMATOGRAPHY A (1998) 827(1), 73–81 8 ‘SEPARATION AND DETERMINATION OF DYES BY ION-PAIR CHROMATOGRAPHY’, BERZASNEVADO J J, GUIBERTEAUCABANILLAS C, CONTENTOSALCEDO A M JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES (1997) 20(18), 3073–3088 9 ‘A COMPARISON OF THREE SPECTROPHOTOMETRIC METHODS FOR SIMULTANEOUS QUANTITATION OF MIXTURES E102 AND E110 FOOD ADDITIVES’, GARCIAPENALVER L, SIMALLORANO J, LOPEZHERNANDEZ J SPECTROSCOPY EUROPE (1999) 11(1), 8–12 10 ‘DETERMINATION OF COLOURANT MATTERS MIXTURES IN FOODS BY SOLID-PHASE SPECTROPHOTOM- ETRY’, CAPITAN F, CAPITANVALLVEY L F, FERNANDEZ M D, DEORBE I, AVIDAD R ANALYTICA CHIMICA ACTA (1996) 331(1), 141–148 11 ‘SPECTROPHOTOMETRIC DETERMINATION OF SINGLE SYNTHETIC FOOD COLOUR IN SOFT DRINKS USING ION-PAIR FORMATION AND EXTRACTION’, LAU O W, POON M M K, MOK S C, WONG F M Y, LUK S F INTERNATIONAL JOURNAL OF FOOD SCIENCE AND TECHNOLOGY (1995) 30(6), 793–798 12 ‘SIMULTANEOUS DETERMINATION OF THE COLORANTS TARTRAZINE, PONCEAU 4R AND SUNSET YELLOW FCF IN FOODSTUFFS BY SOLID PHASE SPECTROPHOTOMETRY USING PARTIAL LEAST SQUARE MULTIVARIATE CALIBRATION’, CAPITANVALLVEY L F, FERNANDEZ M D, DEORBE I, AVIDAD R TALANTA (1998) 47, 861–868 13 ‘FIRST-DERIVATIVE SPECTROPHOTOMETRIC DETERMINATION OF PONCEAU 4R, SUNSET YELLOW AND TARTRAZINE IN CONFECTIONERY PRODUCTS’, SAYAR S, OZDEMIR Y FOOD CHEMISTRY (1998) 61(3), 367–372 14 ‘SIMULTANEOUS SPECTROPHOTOMETRIC DETERMINATION OF MIXTURES OF FOOD COLORANTS’, NI Y G, GONG X F ANALYTICA CHIMICA ACTA (1997) 354(1–3), 163–171 15 ‘RESOLUTION OF TERNARY MIXTURES OF TARTRAZINE, SUNSET YELLOW AND PONCEAU 4R BY DERIVATIVE SPECTROPHOTOMETRIC RATIO SPECTRUM-ZERO CROSSING METHODS IN COMMERCIAL FOODS’, BERZASNEVADO J J, RODRIGUEZFLORES J, GUIBERTEAUCABANILLAS C, VILLASENORLLERENA M J, CONTENTOSALCEDO A M TALANTA (1998), 46(5), 933–942 16 ‘METHOD DEVELOPMENT AND VALIDATION FOR THE SIMULTANEOUS DETERMINATION OF DYES IN FOOD STUFFS BY CAPILLARY ZONE ELECTROPHORESIS’, BERZASNEVADO J J, GUIBERTEAUCABANILLAS C, CONTENTOSALCEDO A M ANALYTICA CHIMICA ACTA (1999) 378(1–3), 63–71 17 ‘SIMULTANEOUS DETERMINATION OF SYNTHETIC FOOD COLOURINGS AND PRESERVATIVES IN BEVER- AGES BY CAPILLARY ZONE ELECTROPHORESIS’, WANG W, HE J H, XU Z, CHEN H M FENXI CESHI XUEBAO (1998) 17(5), 72–75 [CHINESE] 18 ‘HIGH-PERFORMANCE CAPILLARY ELECTROPHORETIC ANALYSIS OF SYNTHETIC FOOD COLORANTS’, KUO K L, HUANG H Y, HSIEH Y Z CHROMATOGRAPHIA (1998) 47(5/6), 249–256 19 ‘DETERMINATION OF SYNTHETIC COLOURS IN CONFECTIONERY BY MICELLAR ELECTROKINETIC CAPILLARY CHROMATOGRAPHY’, THOMPSON C O, TRENERRY V C JOURNAL OF CHROMATOGRAPHY A (1995) 704(1), 195–201 20 ‘SIMULTANEOUS DETERMINATION OF AMARANTH AND SUNSET YELLOW BY RATIO DERIVATIVE VOLTAMMETRY’, NI Y, BAI J TALANTA (1997) 44, 105–109 21 ‘SQUARE WAVE ADSORPTIVE VOLTAMMETRIC DETERMINATION OF SUNSET YELLOW’, NEVADO J J B, FLORE J R, LLERENA M J V TALANTA (1997) 44, 467–474 22 ‘A FLOW-THROUGH SENSOR FOR THE DETERMINATION OF THE DYE SUNSET YELLOW AND ITS SUBSIDIARY SUDAN 1 IN FOODS’, VALENCIA M C, UROZ F, TAFERSITI Y, CAPITAN-VALLVEY L F QUIMICA ANALYTICA (2000) 19(3), 129–134 30–40 µM MOBILE PHASE 60 % SOLUTION B AND 40 % SOLUTION A LINEAR GRADIENT TO 80 % SOLUTION B AND 20 % SOLUTION A AFTER 20 MIN FLOW RATE 1 5 ML/MIN DETECTOR 430 NM SOLUTION A PHOSPHATE BUFFER AND WATER ARE DILUTED 50 ML + 850 ML, AND THIS SOLUTION IS DE-GASSED TO THE DE-GASSED SOLUTION, 50 ML OF CETYLPYRIDINIUM CHLORIDE SOLUTION IS ADDED AND THE FINAL SOLUTION MADE TO 1 L IN A VOLUMETRIC FLASK THE SOLUTION IS DE- GASSED BEFORE THE ADDITION OF CETYLPYRIDINIUM CHLORIDE SOLUTION TO AVOID FROTHING SOLUTION B CETYLPYRIDINIUM CHLORIDE SOLUTION IS DILUTED 50 ML TO 1 L WITH A 1 L + 1 L DILUTION OF ACETONITRILE AND METHANOL E110: SUNSET YELLOW SAMPLE PREPARATION THE SAMPLES WERE PREPARED AS FOLLOWS QUANTITATIVE DETERMINATION BY DIRECT PREPARATION USING CALIBRATION GRAPHS: 5 ML OF THE SAMPLE WAS TRANSFERRED TO A 25 ML FLASK AND DILUTED WITH DEIONISED WATER TO THE MARK GRADIENT PROFILE T0(INITIAL) 20 % ELUENT A, 80 % ELUENT B T1(2 MIN) 100 % ELUENT A T2(4 MIN) 100 % ELUENT A T0(5 MIN) 20 % ELUENT A, 80 % ELUENT B FLOW RATE 2 ML/MIN INJECTION VOLUME 20 µL DETECTION 520 NM GRADIENT ELUTION (1 5 ML/MIN) DIODE-ARRAY GRADIENT ELUTION (2 ML/MIN) 520 NM USING METHANOL AND 0 1 M SODIUM PHOSPHATE BUFFER AT PH ZORBAX ODS GRADIENT ELUTION (1 ML/MIN) 254 NM PHASE HPLC SOY SAUCE AND CENTRIFUGED MEOH–CH3CN–0 02 M- TRIAMMONIUM CITRATE (10:1:39), TO METHANOL (1:1) HPLC BEVERAGES ALTEX ULTRA- GRADIENT ELUTION WITH 0 2 N AND FOODS SPHERE TM ODS AMMONIUM ACETATE AND 18 TO 100 % METHANOL HPLC BEVERAGES NEUTRALISED WITH AQ NH3 AND µBONDAPAK C18 GRADIENT ELUTION (2 ML/MIN) 230 NM FILTERED WITH 20 MM AMMONIUM ACETATE AQ AND METHANOL HIGH-PERFORMANCE DRINKS AND DILUTED WITH WATER AND DIONEX ION GRADIENT ELUTION (1 5 ML/MIN) 480 NM WITH HCL:WATER:ACETONITRILE, CHROMATOGRAPHY POWDER DRINKS 50 µL INJECTION E110: SUNSET YELLOW (B) METHOD MATRIX SAMPLE PREPARATION EXTRACTION DETECTION REFERENCE ION-PAIR HPLC BEVERAGES, DILUTED WITH WATER AND FILTERED NOVA-PAK C18 COLUMN WITH GRADIENT 520 NM GELATINE, SYRUPS ELUTION (1 5 ML/MIN) WITH METHANOL- PHOSPHATE BUFFER OF PH 7 CONTAINING 5 MM TETRA-BUTYLAMMONIUM BROMIDE SPECTRO- COMMERCIALLY DILUTED WITH WATER AND COMPUTER PROGRAM THAT DETERMINES MULTV3 0 QUIMIO PHOTOMETRY VISIBLE AVAILABLE DYES ULTRASONICATED CONCENTRATION OF MIXTURES OF PROGRAM COMPOUNDS BY COMPARING THEIR SPECTRA WITH STANDARD SPECTRA SOLID-PHASE SOFT DRINKS, FILTERED FOOD SAMPLES WERE DILUTED THE MIXTURE WAS AGITATED WITH 50 MG 487 NM SPECTROPHOTOMETRY FRUIT LIQUEURS AND TO 100 ML WITH THE ADDITION OF SEPHADEX DEAE A-25GEL THE SOLID ICE-CREAM 5 ML 1 M ACETATE BUFFER AT PH PHASE WAS EXTRACTED AND PACKED INTO AND 10 ML ETHANOL 1 MM CELLS FOR SPECTROPHOTOMETRIC DETERMINATION SPECTRO- SOFT DRINKS ION-PAIR FORMATION WITH OCTADECYL- EXTRACTION OF THE ION-PAIR INTO 485 NM SOLID-PHASE SOFT DRINKS, SAMPLES DISSOLVED IN WATER AND THE COLOURANTS WERE FIXED IN SEPHADEX BETWEEN 400 AND SPECTROPHOTOMETRY SWEETS AND FRUIT FILTERED DEAE A-25GEL AT PH 2 0 AND PACKED 800 NM PARTIAL LEAST JELLIES INTO 1 MM CELLS FOR SPECTROPHOTOMETRIC SQUARES (PLS) DETERMINATION MULTIVARIATE CALIBRATION USED ANALYTICAL METHODS FOR FOOD ADDITIVES TABLE 1 1 CONT’D (C) METHOD MATRIX SAMPLE PREPARATION METHOD CONDITIONS DETECTION REFERENCE FIRST-DERIVATIVE CONFECTIONERY SAMPLES DILUTED 5–20 G IN 100 ML 350–700 NM FIRST SPECTROPHOTOMETRY PRODUCTS WATER DERIVATIVE SPECTRUM WAS OBTAINED SIMULTANEOUS CANDY AND FOOD SAMPLES WERE DILUTED TO THE COLOURANTS WERE ISOLATED FROM THE 300–700 NM IN 5 NM SPECTROPHOTOMETRY CARBONATED DRINKS 25 ML WITH THE ADDITION OF 5 ML FOOD MATRICES BY SPE USING POLYAMIDE INTERVALS FIRST AND, ACETATE BUFFER AT PH 4 5 AND WATER SORBENT PACKED INTO 1 MM CELLS FOR SECOND DERIVATIVES SPECTROPHOTOMETRIC DETERMINATION WERE ANALYSED BY (PLS) MULTIVARIATE CALIBRATION DERIVATIVE COMMERCIAL THIS METHOD IS APPLIED TO SAMPLES NO SEPARATION STEP IS REQUIRED METHOD SPECTROPHOTOMETRICPRODUCTS CONTAINING 3 DYES TO DETERMINE WAS USED TO DETERMINE SYNTHETIC RATIO SPECTRUM-ZERO EACH DYE UNDER OPTIMUM CONDITIONS MIXTURES OF THESE DYES IN DIFFERENT RATIOS CROSSING FROM 1:1:1 TO 1:5:5 OR EVEN HIGHER CAPILLARY ZONE NON-ALCOHOLIC SAMPLES USED AS IS OR DILUTED WITH A BACKGROUND SOLUTION CONSISTING OF 216 NM ELECTROPHORESIS BEVERAGES AND WATER 15 MM BORATE BUFFER AT PH 10 5, (CZE) FRUIT-FLAVOURED HYDRODYNAMIC INJECTION AND A 20 KV SYRUPS SEPARATION VOLTAGE CZE BEVERAGES – SAMPLE, EITHER CONCENTRATED OR UNCOATED QUARTZ COLUMN OPERATED AT 254 NM STRAWBERRY AND DIRECTLY AFTER FILTRATION WAS APPLIED SEPARATION VOLTAGE 28 KV WITH 10 MM ORANGE DRINKS FOR DETERMINATION BY CZE KH2PO4/NA2B4O7/3 % ETHANOL AT PH AS BACKGROUND ELECTROLYTE E110: SUNSET YELLOW HIGH-PERFORMANCE ICE-CREAM BARS DIRECT INJECTION OF LIQUIDS PH 9 5 BORAX–NAOH BUFFER CONTAINING DIODE-ARRAY CAPILLARY ELECTRO- AND FRUIT SODA 5 MM ?-CYCLODEXTRIN PHORETIC (HPCE) DRINKS MICELLAR ELECTRO- CORDIALS AND 5 G SAMPLE WAS EXTRACTED WITH FUSED-SILICA CAPILLARY COLUMN OPERATED 214 NM KINETIC CAPILLARY CONFECTIONERY 25 ML WATER–METHANOL (4:1) 1 ML AT 30 KV WITH A BUFFER OF 0 05 M SODIUM CHROMATOGRAPHY 0 05 M TETRABUTYLAMMONIUM DEOXYCHOLATE IN 5 MM NAH2PO4/5 MM (MECC) PHOSPHATE WAS ADDED AND EXTRACTED SODIUM BORATE AT PH 8 6/ACETONITRILE BY ADSORPTION ONTO C18 SEP-PAK (17:3) CARTRIDGE AND ELUTION WITH METHANOL RATIO DERIVATIVE SOFT DRINKS SAMPLES WERE DISSOLVED IN WATER, MEASUREMENTS WERE CARRIED OUT DIRECTLY VOLTAMMETRY WARMED TO DISSOLVE COMPLETELY USING AN HMDE (HANGING MERCURY AND FILTERED DROPPING ELECTRODE) SQUARE WAVE REFRESHING DRINKS SAMPLES WERE DILUTED WITH WATER MEASUREMENTS WERE MADE DIRECTLY VOLTAMMETRY BUFFER SOLUTION GAVE AN ADSORPTIVE STRIPPING VOLTAMMETRIC PEAK AT THE HANGING MERCURY DROP ELECTRODE AT: –0 60V USING AN ACCUMULATION POTENTIAL OF –0 40V INTEGRATED SOLID DRINKS SAMPLES (3 ML) INTO A 10 ML WHEN THE FLOW CELL CONTAINS C18 SILICA PHASE SPECTRO- VOLUMETRIC FLASK MADE UP TO THE SUNSET YELLOW IS TRANSPORTED ACROSS PHOTOMETRIC-FIA VOLUME WITH CARRIER SOLUTION AND THE FILLED CELL MEASURING THE ABSORBANCE ANALYSED BY THE FLOW PROCEDURE AT INCREASE AT 487 NM 4 ML/MIN RP-HPLC BITTER PERFORMANCE OF METHOD LINEAR RANGE OF CALIBRATION 2–10 MG/L DETERMINATION LIMIT 4 NG RSD 6 07 % SQUARE OF CORRELATION JELLIES TO 7 REAL SAMPLES (N=5) RSD 1 8–7 6 % FOR COMMERCIAL SAMPLES ORANGE DRINKS: 3 68 MG/L RSD 3 5 % (N=5) PINEAPPLE JELLY: 3 68 MG/L RSD 3 5 % (N=5) ORANGE DRINK: 3 20 MG/L RSD 4 7 % (N=5) HONEY SWEET: 0 19 MG/L RSD 1 8 % (N=5) COLOURANT: 845 0 MG/L RSD 2 5 % (N=5) FRUIT JELLY: 0 66 MG/L RSD 7 6 % (N=5) MELON DRINK: 23 60 MG/L RSD 6 3 % (N=5) IP-HPLC COMMERCIAL PERFORMANCE OF METHOD CALIBRATION GRAPH LINEAR FROM 2–10 MG/L SD 0 071 MG/L PRODUCTS ESTABLISHED WITH STANDARDS RSD 4 22 % DETECTION LIMIT 1 4 NG RECOVERY 99 1 % (N=5) (N=9) AND VALIDATED WITH REAL SAMPLES: BITTER: 16 7±0 3 MG/L COMMERCIAL FOOD PRODUCTS GRENADINE: 29 5±0 3 MG/L GELATINE: 160 0±0 4 MG/KG HPIC DRINKS PERFORMANCE OF METHOD LINEAR RANGE 2 0–40 µG/ML RECOVERIES OF SPIKED SAMPLES ESTABLISHED AND VALIDATED 94 7–109 % (N=4) RSD 2 01 % AT 20 µG/ML (N=7) WITH 3 REAL SAMPLES DETECTION LIMIT 2 0 µG/ML REAL SAMPLES: 42 5±1 0 µG/ML, 67 0±1 4 µG/ML, 176 0±4 0 µG/ML (N=4) E110: SUNSET YELLOW SQUARE WAVE REFRESHING PERFORMANCE OF METHOD CALIBRATION GRAPH LINEAR IN THE RANGE 5–90 µG/L ADSORPTIVE DRINKS ESTABLISHED AND APPLIED TO RSD = 2 2 % FOR A SOLUTION OF 30 µG/L (N=10) IN THE SAME DAY VOLTAMMETRY 3 REAL SAMPLES (N=5) THE DETERMINATION LIMIT WAS 5 µG/L TOF (LEMON) 192±4 µG/L (N=5) GATORADE (LEMON) 5790±116 µG/L (N=5) REFRESHING DRINK (ORANGE) 2142±42 µG/L (N=5) CZE CF NON-ALCOHOLIC PERFORMANCE OF METHOD CALIBRATION GRAPH LINEAR UP TO 4–200 MG/L DETECTION LIMIT 0 38 MG/L BEVERAGES AND ESTABLISHED AND APPLIED RECOVERIES WERE 92 3–111 3 % FOR 4–60 MG/L DYES FROM SYNTHETIC MIXTURES FLAVOURED TO REAL SAMPLES REAL SAMPLES: ICE LOLLY: 11 0±0 2 MG/L BY SYRUPS CZE (N=3) 10 7±0 2 MG/L BY HPLC (N=3) SPECTRO- SOFT DRINKS PERFORMANCE OF METHOD LINEAR RANGE 0–60 µG/ML RECOVERY 99 % (N=6) PHOTOMETRIC ESTABLISHED AND APPLIED TO RSD 1 9 % FOR 8 µG/ML (N=10) REAL SAMPLES SPARKLING ORANGE DRINK: 9 32 µG/ML (N=3) {9 6} RSD 0 1 % RESULTS AGREE WITH MANUFACTURERS’ VALUES {} INTEGRATED DRINKS PERFORMANCE OF METHOD CONCENTRATION RANGE 0 5–20 MG/L DETECTION LIMIT 0 2 MG/L SOLID PHASE ESTABLISHED AND APPLIED TO RSD = 1 6 % SPECTROPHOTO- A REAL SAMPLE MANGO LIQUEUR 39 44±1 334 µG/L (N=3) METRIC-FIA RESULTS FOR SAMPLE COMPARE WITH HPLC DATA FOR THIS SAMPLE DERIVATIVE COMMERCIAL PERFORMANCE OF METHOD CALIBRATION GRAPH LINEAR UP TO 40 MG/L SD 0 8 % AT 8 MG/L SPECTROPHOTO- PRODUCTS ESTABLISHED AND APPLIED RECOVERY 94–105 % METRIC RATIO TO REAL SAMPLES RESULTS FOR SAMPLES COMPARE WITH HPLC DATA FOR THESE SAMPLES SPECTRUM-ZERO CROSSING SP SPECTRO- SOFT DRINKS, PERFORMANCE OF METHOD LINEAR RANGE 15–500 NG/ML DETECTION LIMIT 3 5 NG/ML PHOTOMETRY LIQUEURS, ESTABLISHED AND APPLIED RSD 2 8 % FOR 150 NG/ML ICE-CREAM TO REAL SAMPLES ANALYTICAL METHODS FOR FOOD ADDITIVES TABLE 1 2 CONT’D METHOD MATRIX EXTENT OF VALIDATION STATISTICAL PARAMETERS REFERENCE SPECTRO- COMMERCIAL PERFORMANCE OF METHOD RECOVERY 93 81–106 1 % SD 4 03 MG/L PHOTOMETRIC DYES ESTABLISHED ON STANDARDS RSD 4 0 % FOR 100 MG/L CZE BEVERAGES PERFORMANCE OF METHOD CALIBRATION GRAPH LINEAR RECOVERIES 95–103 % ESTABLISHED AND APPLIED RSD 2 2–5 8 % TO A SOFT DRINK SAMPLE FIRST DERIVATIVE CONFECTIONERY METHOD APPLIED TO 2 REAL RECOVERY 92 1–107 9 % SPECTRO- PRODUCTS SAMPLES (N=5) REAL SAMPLES: SUGAR CANDY: 122 0±1 8 µG/G (N=5) PHOTOMETRY JELLY: 3 2±0 2 µG/G (N=5) RATIO SOFT DRINKS METHOD APPLIED TO (N=3) (N=3) SIMULTANEOUS CANDY AND METHOD APPLIED TO 2 REAL REAL SAMPLES: SOFT DRINK: 13 71 MG/L (N=3) {14 00} SPECTRO- CARBONATED SAMPLES (N=3) CANDY: 8 45 MG/KG (N=3) {8 51} PHOTOMETRY DRINKS RESULTS AGREE WITH MANUFACTURERS’ VALUES {} E110: SUNSET YELLOW HPCE ICE-CREAM BARS METHOD APPLIED TO A REAL CALIBRATION GRAPH LINEAR RSD OF MIGRATION TIME 0 49 % (N=7) AND SODA SAMPLE (N=3) COMMERCIAL SODA DRINK: 9 34 µG/ML RSD 3 81 % (N=3) DRINKS MECC CORDIALS AND METHOD APPLIED TO CALIBRATION GRAPH LINEAR UP TO 100 µG/ML RSD 1 9–4 3 % CONFECTIONERY COMMERCIAL PRODUCTS REPORTING LIMIT 5 MG/KG RESULTS FOR SAMPLES COMPARE WITH HPLC DATA FOR THESE SAMPLES IP-RP-HPLC FRUIT JUICE, METHOD APPLIED TO SOY RECOVERIES 91–113 % CV 0 4–3 7 % SOY SAUCE SAUCE HPLC BEVERAGES METHOD APPLIED TO RECOVERIES 96 7–101 % AND FOODS COMMERCIAL PRODUCTS HPLC BEVERAGES METHOD APPLIED TO RECOVERIES 92–108 % CV 0 4–4 0 % BEVERAGES SAMPLE LEMONADE ANALYTE SUNSET YELLOW NO OF LABORATORIES SAMPLE BITTER KALTY ANALYTE SUNSET YELLOW QUANTIFICATION METHOD DIRECT MEASUREMENT STANDARD ADDITION NUMBER OF DETERMINATIONS STATISTICAL PARAMETERS FOR ASSAY NUMBER OF DETERMINATIONS THE METHOD CONSISTED OF A QUANTITATIVE EXTRACTION, AS ION PAIRS WITH CETYLPYRIDINIUM CHLORIDE, FROM AQUEOUS SOLUTIONS INTO REFERENCES 1 PEARSON’S COMPOSITION AND ANALYSIS OF FOODS, 9 ED KIRK R AND SAWYER R, LONGMAN SCIENTIFIC, HARLOW (1989) 2 ‘DETERMINATION OF SYNTHETIC COAL-TAR DYES IN SOFT DRINKS, SKIMMED MILKS AND CAKES: COLLABORATIVE TRIAL’, DENNIS J, CHAPMAN S, BRERETON P, TURNBULL J, WOOD R J ASSOC PUBL ANALYSTS (1997) 33, 161–202 3 ‘A REVERSE PHASE HPLC METHOD TO DETERMINE SIX FOOD DYES USING BUFFERED MOBILE PHASE’, BERZASNEVADO J J, GUIBERTEAUCABANILLAS C, CONTENTOSALCEDO A M ANALYTICAL LETTERS (1998) 31(14), 2513–2535 4 ‘SEPARATION AND DETERMINATION OF DYES BY ION-PAIR CHROMATOGRAPHY’, 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