聚葡萄糖的FCC（⾷品化学法典）标准
Polydextro
INS: 1200
CAS: [68424-04-4]
DESCRIPTION
Polydextro occurs as an off-white to light tan solid. It is a randomly bonded polymer prepared by the condensation of a melt that consists of approximately 90% D-gluco, 10% sorbitol, and 1% citric acid or 0.1% phosphoric acid on a weight basis. The 1,6-glycosidic linkage predominates in the polymer, but other possible bonds are prent. The product contains small quantities of free gluco, sorbitol, and D-anhydroglucos (levoglucosan), with traces of citric acid or phosphoric acid. It may be partially reduced by transition metal catalytic hydrogenation in an aqueous solution. It may be neutralized with any food-grade ba and decolorized and deionized for further purification. It is very soluble in water.
Function Bulking agent; humectant; texturizer
Packaging and Storage Store in tight, light-proof containers.
IDENTIFICATION
A. P ROCEDURE
Sample solution: 100 mg/mL
Analysis: Add 4 drops of 5% aqueous phenol solution to 1 drop Sample solution, then rapidly add 15 drops of sulfuric acid. Acceptance criterion: A deep yellow to orange color appears.
B. P ROCEDURE
除法的竖式怎么写Sample solution: 100 mg/mL
十二属相表Analysis: While vigorously swirling (vortex mixer), add 1.0 mL of acetone to 1.0 mL of Sample solution. [N OTE: Retain this solution for Identification test C (below).]
Acceptance criterion: The solution remains clear.
C. P ROCEDURE
Analysis: While vigorously swirling, add 2.0 mL of acetone to the retained solution from Identification
test B.
Acceptance criterion: A heavy, milky turbidity develops immediately.
D. P ROCEDURE
Sample solution: 20 mg/mL
Sample: Add 4 mL of alkaline cupric citrate TS to 1 mL of Sample solution. Boil
vigorously for 2 to 4 min. Remove from heat, and allow the precipitate (if any) to
ttle.
Acceptance criterion: The supernatant is blue or blue-green.
ASSAY
P ROCEDURE
Standard stock solution: 0.2 mg/mL -D-gluco
Standard solutions: 50, 40, 20, 10, and 5 µg/mL -D-gluco: made from Standard stock solution
Sample solution: 40 µg/mL: made from Sample stock solution
Phenol solution: Add 20 mL of water to 80 g of phenol.
Analysis: On a daily basis, pipet 2.0 mL of each Standard solution and the Sample solution into parate, acetone-free, 15-mL screw-cap vials. Add 0.12 mL of the
Phenol solution, and mix gently. Uncap each vial and rapidly add 5.0 mL of sulfuric acid. Immediately recap each vial, and shake vigorously. [CAUTION: Wear rubber gloves and a safety shield while adding sulfuric acid. ]
Let the vials stand at room temperature for 45 min, then determine the absorbance of each sample at 490 nm in a suitable spectrophotometer, using a Phenol solution–
sulfuric acid reagent blank in the reference cell. Repeat the procedure three times and obtain the mean absorbance value. For the standard curve, plot mean
absorbance values versus concentrations, in µg/mL, obtained from triplicate
Standard solutions. Calculate the percent polymer by the formula:
1.05[100(A Y)/(S × C) P G 1.11P L]
1.05 = An experimentally derived correction factor to account for the polymer
(which also contains a small amount of sorbitol) not giving the exact amount
of color given by an equivalent amount of gluco monomers
风靡一时的读音
A = Sample absorbance
Y = The y-intercept of the standard curve
S = Slope (approximately 0.02) of absorbance versus gluco concentration,
in g/mL, obtained from the standard curve
C = Concentration (g/mL) of the Sample stock solution, adjusted for ash and
moisture
P G = Percentage of gluco determined under the test for Monomers (below)
P L = Percentage of levoglucosan determined under the test for Monomers
(below)
1.11 = Conversion factor from levoglucosan, which gives an equivalent
amount of color to an equivalent weight of gluco
南阿尔卑斯山Acceptance criterion: NLT 90.0% polymer, calculated on the anhydrous, ash-free basis
IMPURITIES
Change to read:
Inorganic Impurities
L EAD
空调之父[N OTE: For this test, u reagent-grade chemicals with as low a lead content as is
hydrochloric acid, and then rin them thoroughly with high-purity water, preferably obtained from a mixed-bed, strong-acid, strong-ba, ion-exchange cartridge
capable of producing water with an electrical resistivity of 12 to 15 megohms.] Apparatus: U a suitable spectrophotometer (Perkin-Elmer Model 6000, or
equivalent), a graphite furnace containing a L'vov platform (Perkin-Elmer Model
HGA-500, or equivalent), and an autosampler (Perkin-Elmer Model AS-40, or
equivalent). U a lead hollow-cathode lamp (lamp current of 10 mA), a slit width of
0.7 mm (t low), the wavelength t at 283.3 nm, and a deuterium arc lamp for
background correction.
Lead nitrate solution: 100 µg of lead (Pb) ion/mL prepared as follows: Dissolve 159.8 mg of lead nitr
ate in 100 mL of water containing 1 mL of nitric acid. Dilute with water to 1000.0 mL, and mix. Prepare and store this solution in glass containers that are free from lead salts.
Standard stock solution: 10 µg of lead (Pb) ion/mL: from Lead nitrate solution [N OTE: Prepare on the day of u.]
[N OTE: As an alternative to preparing the Lead nitrate solution and Standard stock solution NIST Standard Reference Material containing 10 mg of lead/kg, or equivalent may be ud.]
Standard solutions: 0.02, 0.05, 0.1, and 0.2 µg of lead (Pb) ion/mL: from Standard stock solution
Matrix modifier solution: 10 mg/mL of dibasic ammonium phosphate
Sample solution: Transfer 1 g of sample into a 10-mL volumetric flask, add 5 mL of water, and mix. Dilute to volume, and mix. Spiked sample solution: Prepare a solution as directed under Sample solution, but add 100 µL of the Standard stock solution, dilute to volume, and mix. This solution contains 0.1 µg of lead/mL.
Analysis: With the u of an autosampler, atomize 10-µL aliquots of the four Standard solutions, using the following quence of conditions:
(1) Dry at 130 with a 20-s ramp period, a 40-s
hold time, and a 300-mL/min argon flow rate;
(2) Char at 800 with a 20-s ramp period, a 40-s
Atomize 10 µL of the Matrix modifier solution in combination with either 10 mL of the Sample solution or 10 µL of the Spiked sample solution under identical
conditions ud for the Standard solutions .
Plot a standard curve using the concentration, in µg/mL, of each Standard solution versus its maximum absorbance value compensated for background correction,休闲文学
and draw the best straight line. From the standard curve, determine the
concentrations, C S and C A , in µg/mL, of the Sample solution and the Spiked
sample solution , respectively. Calculate the quantity, in mg/kg, of lead in the
sample taken by the formula:
10C S /W
hold time, and a 300-mL/min argon flow rate;
(3) Atomize at 2400 for 6 s with a 50-mL/min argon flow rate;
(4) Clean at 2600 with a 1-s ramp period, a 5-s hold time, and a 300-mL/min argon flow rate; and
W = Weight (g) of sample taken
弹力产生的条件Calculate the recovery by the formula:
100[(C A C S )/0.1]
0.1 = Amount of lead (µg/mL) added to the Spiked sample solution
Acceptance criterion: NMT 0.5 mg/kg
N ICKEL , Nickel Limit Test ,
Method II , FCC 6 Appendix IIIB (for Hydrogenated Polydextro)
Acceptance criterion: NMT 2 mg/kg
Organic Impurities
5-H YDROXYMETHYLFURFURAL AND R ELATED C OMPOUNDS
Sample solution: 10 mg/mL
Analysis: Read the absorbance of the Sample solution against a water blank at 283 nm in a 1-cm quartz cell in a spectrophotometer. Calculate the percent 5-hydroxymethylfurfural and related compounds by the formula:
(0.749 × A)/C
0.749 = A composite proportionality constant that includes the extinction
coefficient and other molecular weight, unit, and volume conversions
立刻英语A = Absorbance of the Sample solution
C = Concentration (mg/mL) of Sample solution, corrected for ash and
moisture
Acceptance criterion: NMT 0.1%, calculated on the anhydrous, ash-free basis
M ONOMERS
Octadecane solution: 0.5 mg/mL n-octadecane in pyridine
Standard solution: Transfer 50 mg of -D-gluco1, 40 mg of anhydrous D-sorbitol, and 35 mg of D-anhydroglucos, all accurately weighed, into a 100-mL volumetric flask; dissolve in and dilute to volume with pyridine.
Silylated standard solution: Transfer 1.0 mL of Standard solution to a screw-cap vial, and add 1.0 mL of Octadecane solution and 0.5 mL of N-trimethylsilylimidazole. Cap the vial, and immer it in an ultrasonic bath at 70 for 60 min.
Sample solution: Transfer 20 mg of sample into a screw-cap vial, and add 1.0 mL of Octadecane solution, 1 mL of pyridine, and 0.5 mL of N-trimethylsilylimidazole. Cap the vial, and immer it in an ultrasonic bath at 70 for 60 min. Chromatographic system, Appendix IIA
Mode: Gas chromatography
Detector: Flame-ionization detector
Column: 250-cm × 2-mm (id) glass column, or equivalent, packed with 3% OV-1
stationary pha on 100- to 120-mesh Gas Chrom Q, or equivalent
Temperature:
Column: 175
Injection port: 210
Detector: 230
Injection volume: About 3 µL
Analysis: Initially, inject the Silylated standard solution into the gas chromatograph.
Repeat twice, then inject duplicate portions of the Sample solution. [N OTE: Relative retention times (min) are: D-anhydroglucos (levoglucosan), pyrano form (3.7);
furano form (not prent in standard) (4.3); n-octadecane (5.1); -D-gluco (8.7);
D-sorbitol (11.3); -D-gluco (13.3).] Calculate the percentage of each monomer by the formula:
(R × W S)/(R S × W)
R = Ratio of the area of the monomer peak to the area of the octadecane
peak in the sample injection
W S = Weight (mg) of the respective monomer in the Silylated standard
solution
R S = Mean ratio of the area of the monomer peak to the area of the
octadecane peak in the standard injections
W = Weight (mg) of sample taken, adjusted for residue on ignition and
moisture
Acceptance criteria:
D -Anhydroglucos: NMT 4.0%, calculated on the anhydrous, ash-free basis
Gluco and Sorbitol: NMT 6.0%, calculated on the anhydrous, ash-free basis SPECIFIC TESTS
M OLECULAR W EIGHT L IMIT
Mobile pha: Dissolve 35.0 g of sodium nitrate and 1.0 g of sodium azide in 100 mL of HPLC-grade water. Filter through a 0.45-µm filter into a 4-L flask. Dilute to volume with HPLC-grade water. Degas by applying an aspirator vacuum for 30 min. The resulting eluent is 0.1 N sodium nitrate containing 0.025% sodium azide.
Standard solution: Transfer 20 mg each of dextro 2; stachyo 2; and 5800, 23,700, and 100,000 molecular weight (MW) pullulan standards 2 into a 10-mL volumetric flask. Dissolve in and dilute to volume with Mobile pha . Filter through a 0.45-µm syringe filter.
Sample solution: 5 mg/mL in Mobile pha , and filtered through a 0.45-µm filter Chromatographic system, Appendix IIA Mode: High-performance liquid chromatography
Detector: Differential refractometer
Column: Waters Ultrahydrogel 250 A size-exclusion column, or equivalent
Column temperature: 45
Detector cell temperature: 35f
0.1
Flow rate: 0.8 mL/min, reproducible to 0.5%
