USP 39
Official Monographs / Calcium 2879
Chromatographic system
Acceptance criteria: NMT 1.0%
(See Chromatography 〈621〉, System Suitability .)SPECIFIC TESTS
外表英文Mode: Ion chromatography •L OSS ON D RYING 〈731〉
Detector: Conductance Analysis: Dry at 105° for 16 h.Columns
Acceptance criteria
Guard: 4-mm × 5-cm; 15-µm packing L12
Anhydrous: NMT 3.0%
Analytical: 4-mm × 25-cm; 15-µm packing L12Monohydrate: NMT 1.0%, where labeled as intended Anion suppressor: The micromembrane anion sup-for u in preparing injectable dosage forms; NMT
pressor column is connected in ries with the guard 2.0%, where labeled as not intended for u in prepar-and analytical columns. The anion suppressor column ing injectable dosage forms is equipped with a micromembrane that parates Mobile pha from Solution A flowing countercurrent ADDITIONAL REQUIREMENTS
to Mobile pha at a rate of about 7mL/min. [N OTE —•P ACKAGING AND S TORAGE : Prerve in well-clod Condition the system for about 15 min with Mobile containers.
pha at a flow rate of 2mL/min.]•L ABELING : Label it to indicate whether it is anhydrous or Flow rate: 2mL/min monohydrate. Where the quantity of calcium gluconate Injection volume: 50µL is indicated in the labeling of any solution containing System suitability一般将来时态
Calcium Gluconate, this shall be understood to be in Sample: Standard solution terms of anhydrous calcium gluconate (C 12H 22CaO 14).Suitability requirements
Calcium Gluconate intended for u in preparing inject-Column efficiency: NLT 2500 theoretical plates able dosage forms is so labeled. Calcium Gluconate not Tailing factor: NMT 1.2
intended for u in preparing injectable dosage forms is Relative standard deviation: NMT 2.0%so labeled; in addition, it may be labeled also as in-Analysis
tended for u in preparing oral dosage forms.Samples: Standard solution and Sample solution
•USP R EFERENCE S TANDARDS 〈11〉
生活大爆炸5Calculate the percentage of oxalate in the portion of USP Calcium Gluconate Anhydrous RS Calcium Gluconate taken:
USP Calcium Gluconate Monohydrate RS
Result = (r U /r S ) × (C S /C U ) × (M r1/M r2) × F × 100
r U
= peak respon of oxalate from the Sample
solution
r S = peak respon of oxalate from the Standard
Calcium Gluconate Injection
solution
C S = concentration of sodium oxalate in the
DEFINITION
Standard solution (µg/mL)
Calcium Gluconate Injection is a sterile solution of Calcium C U = concentration of Calcium Gluconate in the
Gluconate in Water for Injection. It contains NLT 95.0%Sample solution (mg/mL)
and NMT 105.0% of the labeled amount of total calcium.M r1= molecular weight of oxalate, 88.03The calcium is in the form of calcium gluconate, except M r2= molecular weight of sodium oxalate, 134.00that a small amount may be replaced with an equal
F = conversion factor, 0.001mg/µg amount of calcium in the form of Calcium Saccharate, or Acceptance criteria: NMT 0.01%other suitable calcium salts, for the purpo of stabiliza-•R EDUCIN
G S UBSTANCES
tion. It may contain sodium hydroxide added for adjust-Sample: 1.0g of Calcium Gluconate ment of the pH.
showergelBlank: 20mL of water Injection intended for veterinary u only may be prepared Titrimetric system from Calcium Gluconate solubilized with Boric Acid, or (See Titrimetry 〈541〉.)from Gluconolactone, Boric Acid, and Calcium Carbonate.Mode: Residual titration IDENTIFICATION
Titrant: 0.1 N iodine VS
•A . T HIN -L AYER C HROMATOGRAPHY
Back titrant: 0.1 N sodium thiosulfate VS Standard solution: 10mg/mL of USP Potassium Gluco-Endpoint detection: Visual
nate RS
Analysis: Transfer the Sample to a 250-mL conical flask,Sample solution: Dilute a volume of injection, if neces-dissolve in 20mL of hot water, cool, and add 25mL of sary, with water to obtain a concentration of 10mg/mL alkaline cupric citrate TS. Cover the flask, boil gently for of calcium gluconate.5 min, accurately timed, and cool rapidly to room tem-Chromatographic system
perature. Add 25mL of 0.6 N acetic acid, 10.0mL of (See Chromatography 〈621〉, System Suitability .)Titrant , and 10mL of 3N hydrochloric acid. Titrate with Mode: TLC
the Back titrant , adding 3mL of starch TS as the Adsorbent: 0.25-mm layer of chromatographic silica endpoint is approached. Perform the Blank gel
determination.
Application volume: 5µL
Calculate the percentage of reducing substances (as Developing solvent system: Alcohol, ethyl acetate,dextro) in the Sample taken:
ammonium hydroxide, and water (50:10:10:30)
Result = {[(V B − V S ) × N × F ]/W } × 100
Spray reagent: Dissolve 2.5g of ammonium molyb-date in 50mL of 2N sulfuric acid in a 100-mL volu-V B = Back titrant volume consumed by the Blank
metric flask. Add 1.0g of ceric sulfate, swirl to dis-(mL)
solve, dilute with 2N sulfuric acid to volume, and mix.V S = Back titrant volume consumed by the Sample
Analysis
(mL)
Samples: Standard solution and Sample solution
N = Back titrant normality (mEq/mL)Develop the chromatogram until the solvent front has F = equivalency factor, 27mg/mEq moved about three-fourths of the length of the plate.W
= Sample weight (mg)
Remove the plate from the chamber, and dry at 110°for 20 min. Allow to cool, and spray with the Spray reagent . Heat the plate at 110° for about 10 min.
USP Monographs
2880Calcium / Official Monographs
USP 39
英译汉翻译工具Acceptance criteria: The principal spot of the Sample •USP R EFERENCE S TANDARDS 〈11〉solution corresponds in color, size, and R F value to that USP Endotoxin RS
of the Standard solution .
USP Potassium Gluconate RS
•B . I DENTIFICATION T ESTS —G ENERAL , Calcium 〈191〉
Sample solution: Dilute a volume of Injection with water to obtain a concentration of 20mg/mL of cal-cium gluconate.
Acceptance criteria: Meets the requirements Calcium Gluconate Tablets
ASSAY
DEFINITION
•P ROCEDURE
esd是什么Calcium Gluconate Tablets contain NLT 95.0% and NMT Sample: Accurately measured volume of Injection,105.0% of the labeled amount of calcium gluconate equivalent to 46.5mg of calcium
(C 12H 22CaO 14).
Blank: 150mL of water containing 2mL of 3N hydro-chloric acid
IDENTIFICATION
Titrimetric system •A . I DENTIFICATION T ESTS —G ENERAL , Calcium 〈191〉
(See Titrimetry 〈541〉.)Sample stock solution: A warm, filtered solution in Mode: Direct titration
water, equivalent to 100mg/mL of calcium gluconate Titrant: 0.05 M edetate disodium VS from powdered Tablets
Endpoint detection: Visual
Sample solution: Equivalent to 20mg/mL of calcium Analysis: Add 2mL of 3N hydrochloric acid to the
gluconate from a dilution of the Sample stock solution Sample , and dilute with water to 150mL. Whil
e stirring,Acceptance criteria: Meet the requirements
add 20mL of Titrant from the titration buret. Add •B . T HIN -L AYER C HROMATOGRAPHIC I DENTIFICATION T EST
15mL of 1N sodium hydroxide and 300mg of hy-Standard solution: 10mg/mL of USP Potassium Gluco-droxy naphthol blue, and continue the titration to a nate RS
blue endpoint. Perform a blank determination.
Sample solution: Equivalent to 10mg/mL of calcium Calculate the percentage of the labeled amount of total gluconate from a dilution of the Sample stock solution calcium in the Sample taken:
obtained from Identification test A Chromatographic system
Result = {[(V S − V B ) × M × F ]/W } × 100
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(See Chromatography 〈621〉, Thin-Layer Chromato-graphy .)
V S = Titrant volume consumed by the Sample (mL)Adsorbent: 0.25-mm layer of chromatographic silica V B = Titrant volume consumed by the Blank (mL)gel
M = Titrant molarity (mmol/mL)Application volume: 5µL
F = equivalency factor, 40.08mg/mmol Developing solvent system: Alcohol, ethyl acetate,W = weight of calcium in the Sample (mg)ammonium hydroxide, and water (50:10:10:30)
Acceptance criteria: 95.0%–105.0%
Spray reagent: Dissolve 2.5g of ammonium molyb-date in 50mL of 2N sulfuric acid in a 100-mL volu-SPECIFIC TESTS
metric flask, add 1.0g of ceric sulfate, swirl to dissolve,and dilute with 2N sulfuric acid to volume.Change to read:
Analysis
Samples: Standard solution and Sample solution
•
•B ACTERIAL E NDOTOXINS T EST 〈85〉:•(CN 1-May-2016) NMT
Develop until the solvent front has moved about three-0.17 USP Endotoxin Units/mg of calcium gluconate
fourths of the length of the plate. Remove the plate,and dry at 110° for 20 min. Allow to cool, and spray with Spray reagent. Heat the plate at 110° for about Change to read:
10 min.
Acceptance criteria: The principal spot of the Sample •village什么意思
•P ARTICULATE M ATTER IN I NJECTIONS 〈788〉:•(CN 1-May-2016)
solution corresponds in color, size, and R F value to that Meets the requirements for small-volume injections
of the Standard solution.•P H 〈791〉: 6.0–8.2; 2.5–4.5 where labeled as intended for veterinary u only and as containing boric acid
ASSAY
•P ROCEDURE
Sample: A portion of the powder from NLT 20 finely Change to read:
powdered Tablets, equivalent to 500mg of calcium gluconate
•
•I NJECTIONS AND I MPLANTED D RUG P RODUCTS 〈1〉•(CN 1-May-Blank: Proceed as directed in the Analysis , without the 2016)
: Meets the requirements
Sample .
Titrimetric system ADDITIONAL REQUIREMENTS
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(See Titrimetry 〈541〉.)•P ACKAGING AND S TORAGE : Prerve in single-do contain-Mode: Direct titration
ers, preferably of Type I glass.
Titrant: 0.05 M edetate disodium VS
nice boy
•L ABELING : Label the Injection to indicate its content, if Indicator: Hydroxy naphthol blue, 300mg any, of added calcium salts, calculated as percentage of Endpoint detection: Visual
calcium in the Injection. The label states the total osmo-Analysis: Transfer the Sample to a suitable crucible. Ig-lar concentration in mOsmol/L. Where the contents are nite, gently at first, until free from carbon. Cool the less than 100mL, or where the label states that the Injec-crucible. Add 10mL of water, and dissolve the residue tion is not for direct injection but is to be diluted before by adding sufficient 3N hydrochloric acid, dropwi, to u, the label alternatively may state the total osmolar achieve complete solution. Transfer the solution to a concentration in mOsmol/mL. The labeling indicates that suitable container, and add about 150mL of water.the Injection must be clear at the time of u, and that if While stirring, preferably with a magnetic stirrer, add crystallization has occurred, warming may redissolve the 20mL of Titrant from a 50-mL buret. Add 15mL of 1N precipitate. Injection intended for veterinary u only is sodium hydroxide, then add the Indicator . Continue the so labeled. If Injection contains boric acid, it is so labeled.
titration to a blue endpoint. Perform a Blank determination.
U S P M o n o g r a p h s
