美国药典USP32测试溶液配制

TEST SOLUTIONS (TS)

Certain of the following test solutions are intended for use as acid-base indicators in volumetric analyses. Such solutions should be so adjusted that when 0.15 mL of the indicator solution is added to 25 mL of carbon

dioxide-free water, 0.25 mL of 0.02 N acid or alkali, respectively, will produce the characteristic color change. Similar solutions are intended for use in pH measurement. Where no special directions for their preparation are given, the same solution is suitable for both purposes.

Where it is directed that a volumetric solution be used as the test solution, standardization of the solution used as TS is not required.

In general, the directive to prepare a solution ―fresh‖ indicates that the solution is of limited stability and must be prepared on the day of use.

For the preparation of Test Solutions, use reagents of the quality described under Reagents.

Acetaldehyde TS —Mix 4 mL of acetaldehyde, 3 mL of alcohol, and 1 mL of water. Prepare this solution fresh.

Acetate Buffer TS —Dissolve 320 g of ammonium acetate in 500 mL of water, add 5 mL of glacial acetic acid, dilute with water to 1000.0 mL, and mix. This solution has a pH between 5.9 and 6.0.

Acetic Acid, Glacial, TS —Determine the water content of a specimen of glacial acetic acid by the Titrimetric Method (see Water Determination 921). If the acid contains more than 0.05% of water, add a few mL of acetic anhydride, mix, allow to stand overnight, and again determine the water content. If the acid contains less than 0.02% of water, add sufficient water to make the final concentration between 0.02% and 0.05%, mix, allow to stand overnight, and again determine the water content. Repeat the adjustment with

acetic anhydride or water, as necessary, until the resulting solution shows a water content between 0.02% and 0.05%.

Acetic Acid, Strong, TS —Add 300.0 mL of glacial acetic acid, and dilute with water to 1000 mL. This solution contains about 30% (v/v) of CH3COOH and has a concentration of about 5 N.

Acetic Acid–Ammonium Acetate Buffer TS —Dissolve 77.1 g of ammonium acetate in water, add 57 mL of glacial acetic acid, and dilute with water to 1000 mL.

Acetone, Buffered, TS —Dissolve 8.15 g of sodium acetate and 42 g of sodium chloride in about 100 mL of water, and add 68 mL of 0.1 N hydrochloric acid and 150 mL of acetone. Mix, and dilute with water to 500 mL.

Acid Ferric Chloride TS —Mix 60 mL of glacial acetic acid with 5 mL of sulfuric acid, add 1 mL of ferric chloride TS, mix, and cool.

Acid Ferrous Sulfate TS —See Ferrous Sulfate, Acid, TS.

Acid Stannous Chloride TS —See Stannous Chloride, Acid, TS.

Acid Stannous Chloride TS, Stronger —See Stannous Chloride, Acid, TS.

Albumen TS —Carefully separate the white from the yolk of a strictly fresh hen's egg. Shake the white with 100 mL of water until mixed and all but the chalaza has undergone solution; then filter. Prepare the solution fresh.

Alcohol–Phenol TS —Dissolve 780 mg of phenol in alcohol to make 100 mL.

Alcoholic Ammonia TS —See Ammonia TS, Alcoholic.

Alcoholic Mercuric Bromide TS —See Mercuric Bromide TS, Alcoholic.

Alcoholic Potassium Hydroxide TS —See Potassium Hydroxide TS, Alcoholic.

Alkaline Cupric Citrate TS —See Cupric Citrate TS, Alkaline.

Alkaline Cupric Citrate TS 2 —See Cupric Citrate TS 2, Alkaline.

Alkaline Cupric Iodide TS —See Cupric Iodide TS, Alkaline.

Alkaline Cupric Tartrate TS (Fehling's Solution)—See Cupric Tartrate TS, Alkaline.

Alkaline Mercuric–Potassium Iodide TS —See Mercuric–Potassium Iodide TS, Alkaline.

Alkaline Picrate TS —See Picrate TS, Alkaline.

Alkaline Sodium Hydrosulfite TS —See Sodium Hydrosulfite TS, Alkaline. Amaranth TS —Dissolve 20 mg of amaranth in 10 mL of water.

Aminonaphtholsulfonic Acid TS —Accurately weigh 5 g of sodium sulfite, 94.3 g of sodium bisulfite, and 700 mg of 1,2,4-aminonaphtholsulfonic acid, and mix. Prepare aminonaphtholsulfonic acid TS fresh on the day of use by dissolving 1.5 g of the dry mixture in 10 mL of water.

Ammonia–Ammonium Chloride Buffer TS —Dissolve 67.5 g of ammonium chloride in water, add 570 mL of ammonium hydroxide, and dilute with water to 1000 mL.

Ammonia–Cyanide TS —Dissolve 2 g of potassium cyanide in 15 mL of ammonium hydroxide, and dilute with water to 100 mL.

Ammonia TS —It contains between 9.5% and 10.5% of NH3. Prepare by diluting 350 mL of Ammonia Water, Stronger (see in the section, Reagents) with water to make 1000 mL.

Ammonia TS, Alcoholic —A solution of ammonia gas in alcohol. Clear, colorless liquid having a strong odor of ammonia. Specific gravity: about 0.80. It contains between 9% and 11% of NH3. Store it in alkali-resistant containers, in a cold place.

Ammonia TS, Stronger —Use Ammonia Water, Stronger (see in the section Reagents).

Ammoniacal Potassium Ferricyanide TS —Dissolve 2 g of potassium ferricyanide in 75 mL of water, add 25 mL of ammonium hydroxide, and mix.

Ammoniated Cupric Oxide TS —See Cupric Oxide, Ammoniated, TS.

Ammonium Acetate TS —Dissolve 10 g of ammonium acetate in water to make 100 mL.

Ammonium Carbonate TS —Dissolve 20 g of ammonium carbonate and 20 mL of ammonia TS in water to make 100 mL.

Ammonium Chloride TS —Dissolve 10.5 g of ammonium chloride in water to make 100 mL.

Ammonium Chloride–Ammonium Hydroxide TS —Mix equal volumes of water and ammonium hydroxide, and saturate with ammonium chloride.

Ammonium Molybdate TS —Dissolve 6.5 g of finely powdered molybdic acid in a mixture of 14 mL of water and 14.5 mL of ammonium hydroxide. Cool the solution, and add it slowly, with stirring, to a well-cooled mixture of 32 mL of nitric acid and 40 mL of water. Allow to stand for 48 hours, and filter through a fine-porosity, sintered-glass crucible. This solution deteriorates upon standing and is unsuitable for use if, upon the addition of 2 mL of dibasic sodium phosphate TS to 5 mL of the solution, an abundant yellow precipitate does not form at once or after slight warming. Store it in the dark. If a precipitate forms during storage, use only the clear supernatant.

Ammonium Oxalate TS —Dissolve 3.5 g of ammonium oxalate in water to make 100 mL.

Ammonium Phosphate, Dibasic, TS (Ammonium Phosphate TS)— Dissolve 13 g of dibasic ammonium phosphate in water to make 100 mL.

Ammonium Polysulfide TS —Yellow liquid, made by saturating ammonium sulfide TS with sulfur.

Ammonium Pyrrolidinedithiocarbamate, Saturated, TS —Add about 10 g of ammonium pyrrolidinedithiocarbamate to a 1000-mL volumetric flask, and dilute with water to volume.

Ammonium Reineckate TS —Shake about 500 mg of ammonium reineckate with 20 mL of water frequently during 1 hour, and filter. Use within 2 days.

Ammonium Sulfide TS —Saturate ammonia TS with hydrogen sulfide by bubbling hydrogen sulfide gas through the solution for 1 minute. This solution must be freshly prepared. The solution is not rendered turbid either by magnesium sulfate TS or by calcium chloride TS (carbonate). This solution is unstable for use if an abundant precipitate of sulfur is present.

Residue on ignition: not more than 0.05%.

Ammonium Thiocyanate TS —Dissolve 8 g of ammonium thiocyanate in water to make 100 mL.

Ammonium Vanadate TS —Dissolve 2.5 g of ammonium vanadate in 500 mL of boiling water, cool, and add 20 mL of nitric acid. Mix, cool, and add water to make 1 L. Store in polyethylene containers.

Anthrone TS —Within 12 hours of use, rapidly dissolve 35 mg of anthrone in a hot mixture of 35 mL of water and 65 mL of sulfuric acid. Immediately cool in an ice bath to room temperature, and filter through glass wool. Allow the solution to stand at room temperature for 30 minutes before use.

Antimony Trichloride TS —Dissolve 20 g of antimony trichloride in chloroform to make 100 mL. Filter if necessary.

Barium Chloride TS —Dissolve 12 g of barium chloride in water to make 100 mL.

Barium Hydroxide TS —A saturated solution of barium hydroxide in recently boiled water. Prepare the solution fresh.

Barium Nitrate TS —Dissolve 6.5 g of barium nitrate in water to make 100 mL.

Betanaphthol TS —See 2-Naphthol TS.

Biuret Reagent TS —Dissolve 1.5 g of cupric sulfate and 6.0 g of potassium sodium tartrate in 500 mL of water in a 1000-mL volumetric flask. Add 300 mL of carbonate-free sodium hydroxide solution (1 in 10), dilute with

carbonate-free sodium hydroxide solution (1 in 10) to 1000 mL, and mix.

Blue Tetrazolium TS —Dissolve 500 mg of blue tetrazolium in alcohol to make 100 mL.

Brilliant Blue G TS —Transfer 25 mg of brilliant blue G to a 100-mL volumetric flask, add 12.5 mL of alcohol and 25 mL of phosphoric acid, dilute with water to volume, and mix.

Bromine TS (Bromine Water)— A saturated solution of bromine, prepared by agitating 2 to 3 mL of bromine with 100 mL of cold water in a glass-stoppered bottle, the stopper of which should be lubricated with petrolatum. Store it in a cold place, protected from light.

Bromine–Sodium Acetate TS —Dissolve 100 g of sodium acetate in 1000 mL of glacial acetic acid, add 50 mL of bromine, and mix.

p-Bromoaniline TS —Add 8 g of p-bromoaniline to a mixture of 380 mL of

thiourea-saturated glacial acetic acid, 10 mL of sodium chloride solution (1 in 5), 5 mL of oxalic acid solution (1 in 20), and 5 mL of dibasic sodium phosphate solution (1 in 10) in a low-actinic glass bottle. Mix, and allow to stand overnight before using. Protect from light, and use within 7 days.

Bromocresol Blue TS —Use Bromocresol Green TS.

Bromocresol Green TS —Dissolve 50 mg of bromocresol green in 100 mL of alcohol, and filter if necessary.

Bromocresol Green–Methyl Red TS —Dissolve 0.15 g of bromocresol green and 0.1 g of methyl red in 180 mL of alcohol, and dilute with water to 200 mL.

Bromocresol Purple TS —Dissolve 250 mg of bromocresol purple in 20 mL of 0.05 N sodium hydroxide, and dilute with water to 250 mL.

Bromophenol Blue TS —Dissolve 100 mg of bromophenol blue in 100 mL of diluted alcohol, and filter if necessary.

Bromothymol Blue TS —Dissolve 100 mg of bromothymol blue in 100 mL of diluted alcohol, and filter if necessary.

Buffered Acetone TS —See Acetone, Buffered, TS.

Calcium Chloride TS —Dissolve 7.5 g of calcium chloride in water to make 100 mL.

Calcium Hydroxide TS —Use Calcium Hydroxide Topical Solution (USP monograph).

Calcium Sulfate TS —A saturated solution of calcium sulfate in water.

Ceric Ammonium Nitrate TS —Dissolve 6.25 g of ceric ammonium nitrate in 10 mL of 0.25 N nitric acid. Use within 3 days.

Chloral Hydrate TS —Dissolve 50 g of chloral hydrate in a mixture of 15 mL of water and 10 mL of glycerin.

Chlorine TS (Chlorine Water)— A saturated solution of chlorine in water. Place the solution in small, completely filled, light-resistant containers. Chlorine TS, even when kept from light and air, is apt to deteriorate. Store it in a cold, dark place. For full strength, prepare this solution fresh.

Chromotropic Acid TS —Dissolve 50 mg of chromotropic acid or its disodium salt in 100 mL of 75% sulfuric acid, which may be made by cautiously adding 75 mL of sulfuric acid to 33.3 mL of water.

Cobalt–Uranyl Acetate TS —Dissolve, with warming, 40 g of uranyl acetate in a mixture of 30 g of glacial acetic acid and sufficient water to make 500 mL. Similarly, prepare a solution containing 200 g of cobaltous acetate in a mixture of 30 g of glacial acetic acid and sufficient water to make 500 mL. Mix the two solutions while still warm, and cool to 20. Maintain the temperature at 20for about 2 hours to separate the excess salts from solution, and then pass through a dry filter.

Cobaltous Chloride TS —Dissolve 2 g of cobaltous chloride in 1 mL of hydrochloric acid and sufficient water to make 100 mL.

Congo Red TS —Dissolve 500 mg of congo red in a mixture of 10 mL of alcohol and 90 mL of water.

m-Cresol Purple TS —Dissolve 0.10 g of metacresol purple in 13 mL of 0.01 N sodium hydroxide, dilute with water to 100 mL, and mix.

Cresol Red TS —Triturate 100 mg of cresol red in a mortar with 26.2 mL of 0.01 N sodium hydroxide until solution is complete, then dilute the solution with water to 250 mL.

Cresol Red–Thymol Blue TS —Add 15 mL of thymol blue TS to 5 mL of cresol red TS, and mix.

Crystal Violet TS —Dissolve 100 mg of crystal violet in 10 mL of glacial acetic acid.

Cupric Acetate TS —Dissolve 100 mg of cupric acetate in about 5 mL of water to which a few drops of acetic acid have been added. Dilute to 100 mL, and filter, if necessary.

Cupric Acetate TS, Stronger (Barfoed's Reagent)— Dissolve 13.3 g of cupric acetate in a mixture of 195 mL of water and 5 mL of acetic acid.

Cupric-Ammonium Sulfate TS —To cupric sulfate TS add ammonia TS, dropwise, until the precipitate initially formed is nearly but not completely dissolved. Allow to settle, and decant the clear solution. Prepare this solution fresh.

Cupric Citrate TS —Dissolve 25 g of cupric sulfate, 50 g of citric acid, and 144 g of anhydrous sodium carbonate in water, and dilute with water to 1000 mL.

Cupric Citrate TS, Alkaline —With the aid of heat, dissolve 173 g of dihydrated sodium citrate and 117 g of monohydrated sodium carbonate in about 700 mL of water, and filter through paper, if necessary, to obtain a clear solution. In a separate container dissolve 17.3 g of cupric sulfate in about 100 mL of water, and slowly add this solution, with constant stirring, to the first solution. Cool the mixture, add water to make 1000 mL, and mix.

Cupric Citrate TS 2, Alkaline —With the aid of heat, dissolve about 173 g of sodium citrate dihydrate and 117 g of sodium carbonate monohydrate in about 700 mL of water, and filter. In a second flask, dissolve about 27.06 g of cupric sulfate (Cu2O4·5H2O) in about 100 mL of water. Slowly combine the two solutions while stirring, and dilute with water to 1000 mL.

Cupric Iodide TS, Alkaline —Dissolve 7.5 g of cupric sulfate (CuSO4·5H2O) in about 100 mL of water. In a separate container dissolve 25 g of anhydrous sodium carbonate, 20 g of sodium bicarbonate, and 25 g of potassium sodium tartrate in about 600 mL of water. With constant stirring, add the cupric sulfate solution to the bottom of the alkaline tartrate solution by means of a funnel that touches the bottom of the container. Add 1.5 g of potassium iodide, 200 g of anhydrous sodium sulfate, 50 to 150 mL of 0.02 M potassium iodate, and sufficient water to make 1000 mL.

Cupric Oxide, Ammoniated, TS (Schweitzer's Reagent)—Dissolve 10 g of cupric sulfate in 100 mL of water, add sufficient sodium hydroxide solution (1 in 5) to precipitate the copper hydroxide, collect the latter on a filter, and wash free from sulfate with cold water. Dissolve the precipitate, which must be kept

wet during the entire process, in the minimum quantity of ammonia TS necessary for complete solution.

Cupric Sulfate TS —Dissolve 12.5 g of cupric sulfate in water to make 100 mL.

Cupric Tartrate TS, Alkaline (Fehling's Solution)—

The Copper Solution (A)— Dissolve 34.66 g of carefully selected, small crystals of cupric sulfate, showing no trace of efflorescence of adhering moisture, in water to make 500 mL. Store this solution in small, tight containers.

The Alkaline Tartrate Solution (B)— Dissolve 173 g of crystallized potassium sodium tartrate and 50 g of sodium hydroxide in water to make 500 mL. Store this solution in small, alkali-resistant containers.

For use, mix exactly equal volumes of Solutions A and B at the time required.

Delafield's Hematoxylin TS —Prepare 400 mL of a saturated solution of ammonium alum (Solution A). Dissolve 4 g of hematoxylin in 25 mL of alcohol, mix it with Solution A, and allow it to stand for 4 days in a flask closed with a pledget of purified cotton and exposed to light and air (Solution B). Then filter Solution B, and add to it a Solution C consisting of a mixture of 100 mL of glycerin and 100 mL of methanol. Mix, and allow the mixture to stand in a warm place, exposed to light, for 6 weeks until it becomes dark-colored. Store in tightly stoppered bottles.

For use in staining endocrine tissue, dilute this test solution with an equal volume of water.

Denigès' Reagent —See Mercuric Sulfate TS.

Diazobenzenesulfonic Acid TS —Place in a beaker 1.57 g of sulfanilic acid,

previously dried at 105for 3 hours, add 80 mL of water and 10 mL of diluted hydrochloric acid, and warm on a steam bath until dissolved. Cool to 15 (some of the sulfanilic acid may separate but will dissolve later), and add slowly, with constant stirring, 6.5 mL of sodium nitrite solution (1 in 10). Then dilute with water to 100 mL.

Dichlorofluorescein TS —Dissolve 100 mg of dichlorofluorescein in 60 mL of alcohol, add 2.5 mL of 0.1 N sodium hydroxide, mix, and dilute with water to 100 mL.

2,7-Dihydroxynaphthalene TS —Dissolve 100 mg of

2,7-dihydroxynaphthalene in 1000 mL of sulfuric acid, and allow the solution to stand until the yellow color disappears. If the solution is very dark, discard it and prepare a new solution from a different supply of sulfuric acid. This solution is stable for approximately 1 month if stored in a dark bottle.

Diiodofluorescein TS —Dissolve 500 mg of diiodofluorescein in a mixture of 75 mL of alcohol and 30 mL of water.

Diluted Lead Subacetate TS —See Lead Subacetate TS, Diluted.

p-Dimethylaminobenzaldehyde TS —Dissolve 125 mg of

p-dimethylaminobenzaldehyde in a cooled mixture of 65 mL of sulfuric acid and 35 mL of water, and add 0.05 mL of ferric chloride TS. Use within 7 days.

Dinitrophenylhydrazine TS —Carefully mix 10 mL of water and 10 mL of sulfuric acid, and cool. To the mixture, contained in a glass-stoppered flask, add 2 g of 2,4-dinitrophenylhydrazine, and shake until dissolved. To the solution add 35 mL of water, mix, cool, and filter.

Diphenylamine TS —Dissolve 1.0 g of diphenylamine in 100 mL of sulfuric acid. The solution should be colorless.

Diphenylcarbazone TS —Dissolve 1 g of crystalline diphenylcarbazone in 75 mL of alcohol, then add alcohol to make 100 mL. Store in a brown bottle.

Dithizone TS —Dissolve 25.6 mg of dithizone in 100 mL of alcohol. Store in a cold place, and use within 2 months.

Dragendorff's TS —Mix 850 mg of bismuth subnitrate with 40 mL of water and 10 mL of glacial acetic acid (Solution A). Dissolve 8 g of potassium iodide in 20 mL of water (Solution B). Mix equal portions of Solution A and Solution B to obtain a stock solution, which can be stored for several months in a dark bottle. Mix 10 mL of the stock solution with 20 mL of glacial acetic acid, and dilute with water to make 100 mL.

Edetate Disodium TS —Dissolve 1 g of edetate disodium in 950 mL of water, add 50 mL of alcohol, and mix.

Eosin Y TS (adsorption indicator)—Dissolve 50 mg of eosin Y in 10 mL of water.

Eriochrome Black TS —Dissolve 200 mg of eriochrome black T and 2 g of hydroxylamine hydrochloride in methanol to make 50 mL.

Eriochrome Cyanine TS —Dissolve 750 mg of eriochrome cyanine R in 200 mL of water, add 25 g of sodium chloride, 25 g of ammonium nitrate, and 2 mL of nitric acid, and dilute with water to 1000 mL.

Fehling's Solution —See Cupric Tartrate TS, Alkaline.

Ferric Ammonium Sulfate TS —Dissolve 8 g of ferric ammonium sulfate in water to make 100 mL.

Ferric Chloride TS —Dissolve 9 g of ferric chloride in water to make 100 mL.

Ferroin TS —Dissolve 0.7 g of ferrous sulfate and 1.76 g of o-phenanthroline monohydrochloride monohydrate in water, and dilute with water to 100 mL.

Ferrous Sulfate TS —Dissolve 8 g of clear crystals of ferrous sulfate in about 100 mL of recently boiled and thoroughly cooled water. Prepare this solution fresh.

Ferrous Sulfate, Acid, TS —Dissolve 7 g of ferrous sulfate crystals in 90 mL of recently boiled and thoroughly cooled water, and add sulfuric acid to make 100 mL. Prepare this solution immediately prior to use.

Folin-Ciocalteu Phenol TS —Into a 1500-mL flask introduce 100 g of sodium tungstate, 25 g of sodium molybdate, 700 mL of water, 50 mL of phosphoric acid, and 100 mL of hydrochloric acid. Gently reflux the mixture for about 10 hours, and add 150 g of lithium sulfate, 50 mL of water, and a few drops of bromine. Boil the mixture, without the condenser, for about 15 minutes, or until the excess bromine is expelled. Cool, dilute with water to 1 L, and filter: the filtrate has no greenish tint. Before use, dilute 1 part of the filtrate with 1 part of water. When used for protein determination (i.e., Lowry assay), this reagent must be further diluted (1:5) with water. See Method 2 in Total Protein Assay under Biotechnology-Derived Articles—Total Protein Assay 1057.

Formaldehyde TS —Use Formaldehyde Solution (see in the section Reagents).

Fuchsin–Pyrogallol TS —Dissolve 100 mg of basic fuchsin in 50 mL of water that previously has been boiled for 15 minutes and allowed to cool slightly. Cool, add 2 mL of a saturated solution of sodium bisulfite, mix, and allow to stand for not less than 3 hours. Add 0.9 mL of hydrochloric acid, mix, and allow to stand overnight. Add 100 mg of pyrogallol, shake until solution is effected, and dilute with water to 100 mL. Store in an amber-colored glass bottle in a refrigerator.

Fuchsin–Sulfurous Acid TS —Dissolve 200 mg of basic fuchsin in 120 mL of hot water, and allow the solution to cool. Add a solution of 2 g of anhydrous sodium sulfite in 20 mL of water, then add 2 mL of hydrochloric acid. Dilute the solution with water to 200 mL, and allow to stand for at least 1 hour. Prepare this solution fresh.

Gastric Fluid, Simulated, TS —Dissolve 2.0 g of sodium chloride and 3.2 g of purified pepsin, that is derived from porcine stomach mucosa, with an activity of 800 to 2500 units per mg of protein, in 7.0 mL of hydrochloric acid and sufficient water to make 1000 mL. [note—Pepsin activity is described in the Food Chemicals Codex specifications under General Tests and Assays.] This test solution has a pH of about 1.2.

Gelatin TS (for the assay of Corticotropin Injection)—Dissolve 340 g of

acid-treated precursor gelatin (Type A) in water to make 1000 mL. Heat the solution in an autoclave at 115for 30 minutes after the exhaust line

temperature has reached 115. Cool the solution, and add 10 g of phenol and 1000 mL of water. Store in tight containers in a refrigerator.

Glacial Acetic Acid TS —See Acetic Acid, Glacial, TS.

Glucose Oxidase–Chromogen TS —A solution containing, in each mL, 0.5

μmol of 4-aminoantipyrine, 22.0 μmol of sodium p-hydroxybenzoate, not less than 7.0 units of glucose oxidase, and not less than 0.5 units of peroxidase, and buffered to a pH of 7.0 ± 0.1.

Suitability —When used for determining glucose in Inulin, ascertain that no significant color results by reaction with fructose, and that a suitable absorbance-versus-concentration slope is obtained with glucose.

[note—A suitable grade is available, as a concentrate, from Worthington Diagnostics, Division of Millipore Corp., https://www.wendangku.net/doc/ee15351245.html,.]

Glycerin Base TS —To 200 g of glycerin add water to bring the total weight to 235 g. Add 140 mL of 1 N sodium hydroxide and 50 mL of water.

Gold Chloride TS —Dissolve 1 g of gold chloride in 35 mL of water.

Hydrogen Peroxide TS —Use Hydrogen Peroxide Topical Solution (USP monograph).

Hydrogen Sulfide TS —A saturated solution of hydrogen sulfide, made by passing H2S into cold water. Store it in small, dark amber-colored bottles, filled nearly to the top. It is unsuitable unless it possesses a strong odor of H2S, and unless it produces at once a copious precipitate of sulfur when added to an equal volume of ferric chloride TS. Store in a cold, dark place.

Hydroxylamine Hydrochloride TS —Dissolve 3.5 g of hydroxylamine hydrochloride in 95 mL of 60% alcohol, and add 0.5 mL of bromophenol blue solution (1 in 1000 of alcohol) and 0.5 N alcoholic potassium hydroxide until a greenish tint develops in the solution. Then add 60% alcohol to make 100 mL.

8-Hydroxyquinoline TS —Dissolve 5 g of 8-hydroxyquinoline in alcohol to make 100 mL.

Indigo Carmine TS (Sodium Indigotindisulfonate TS)— Dissolve a quantity of sodium indigotindisulfonate, equivalent to 180 mg of C16H8N2O2(SO3Na)2, in water to make 100 mL. Use within 60 days.

Indophenol–Acetate TS (for the assay of Corticotropin Injection)—To 60 mL of standard dichlorophenol-indophenol solution (see in the section Volumetric Solutions) add water to make 250 mL. Add to the resulting solution an equal volume of sodium acetate solution freshly prepared by dissolving 13.66 g of anhydrous sodium acetate in water to make 500 mL and adjusting with 0.5 N acetic acid to a pH of 7. Store in a refrigerator, and use within 2 weeks.

Intestinal Fluid, Simulated, TS —Dissolve 6.8 g of monobasic potassium phosphate in 250 mL of water, mix, and add 77 mL of 0.2 N sodium hydroxide and 500 mL of water. Add 10.0 g of pancreatin, mix, and adjust the resulting solution with either 0.2 N sodium hydroxide or 0.2 N hydrochloric acid to a pH of 6.8 ± 0.1. Dilute with water to 1000 mL.

Iodine TS —Use 0.1 N Iodine (see in the section Volumetric Solutions).

Iodine, Diluted TS— Transfer 10.0 mL of 0.1 N iodine VS to a 100-mL volumetric flask, dilute with water to volume, and mix.

Iodine Monochloride TS —Dissolve 10 g of potassium iodide and 6.44 g of potassium iodate in 75 mL of water in a glass-stoppered container. Add 75 mL of hydrochloric acid and 5 mL of chloroform, and adjust to a faint iodine color (in the chloroform) by adding dilute potassium iodide or potassium iodate solution. If much iodine is liberated, use a stronger solution of potassium iodate than 0.01 M at first, making the final adjustment with the 0.01 M potassium iodate. Store in a dark place, and readjust to a faint iodine color as necessary.

Iodine and Potassium Iodide TS 1 —Dissolve 500 mg of iodine and 1.5 g of potassium iodide in 25 mL of water.

Iodine and Potassium Iodide TS 2 —Dissolve 12.7 g of iodine and 20 g of potassium iodide in water, and dilute with water to 1000.0 mL. To 10.0 mL of this solution, add 0.6 g of potassium iodide, and dilute with water to 100.0 mL. Prepare immediately before use.

Iodobromide TS —Dissolve 20 g of iodine monobromide in glacial acetic acid to make 1000 mL. Store in glass containers, protected from light.

Iodochloride TS —Dissolve 16.5 g of iodine monochloride in 1000 mL of glacial acetic acid.

Iodoplatinate TS —Dissolve 300 mg of platinic chloride in 97 mL of water. Immediately prior to use, add 3.5 mL of potassium iodide TS, and mix.

Iron–Phenol TS (Iron-Kober Reagent)— Dissolve 1.054 g of ferrous ammonium sulfate in 20 mL of water, and add 1 mL of sulfuric acid and 1 mL of 30 percent hydrogen peroxide. Mix, heat until effervescence ceases, and dilute

with water to 50 mL. To 3 volumes of this solution contained in a volumetric flask add sulfuric acid, with cooling, to make 100 volumes. Purify phenol by distillation, discarding the first 10% and the last 5%, collecting the distillate, with exclusion of moisture, in a dry, tared glass-stoppered flask of about twice the volume of the phenol. Solidify the phenol in an ice bath, breaking the top crust with a glass rod to ensure complete crystallization. Weigh the flask and its contents, add to the phenol 1.13 times its weight of the iron–sulfuric acid solution prepared as directed, insert the stopper in the flask, and allow to stand, without cooling but with occasional mixing, until the phenol is liquefied. Shake the mixture vigorously until mixed, allow to stand in the dark for 16 to 24 hours, and again weigh the flask and its contents. To the mixture add 23.5% of its weight of a solution of 100 volumes of sulfuric acid in 110 volumes of water, mix, transfer to dry glass-stoppered bottles, and store in the dark, protected from atmospheric moisture. Use within 6 months. Dispense the reagent from a small-bore buret, arranged to exclude moisture, capable of delivering 1 mL in 30 seconds or less, and having no lubricant, other than reagent, on its stopcock. Wipe the buret tip with tissue before each addition.

Iron Salicylate TS —Dissolve 500 mg of ferric ammonium sulfate in 250 mL of water containing 10 mL of diluted sulfuric acid, and add water to make 500 mL. To 100 mL of the resulting solution add 50 mL of a 1.15% solution of sodium salicylate, 20 mL of diluted acetic acid, and 80 mL of a 13.6% solution of sodium acetate, then add water to make 500 mL. Store in a well-closed container. Protect from light. Use within 2 weeks.

Lead Acetate TS —Dissolve 9.5 g of clear, transparent crystals of lead acetate in recently boiled water to make 100 mL. Store in well-stoppered bottles.

溶出度检查法美国药典USP-711

<711> DISSOLUTION 溶出度 (USP39-NF34 Page 540) General chapter Dissolution <711> is being harmonized with the corresponding texts of the European Pharmacopoeia and/or the Japanese Pharmacopoeia. These pharmacopeias have undertaken to not make any unilateral change to this harmonized chapter. 通则<711>溶出度与欧盟药典和日本药典中的相应部分相统一。这三部药典承诺不做单方面的修改。 Portions of the present general chapter text that are national USP text, and therefore not part of the harmonized text, are marked with symbols to specify this fact. 本章中的部分文字为本国USP内容，并没有与其他药典统一。此部分以（）标注。 This test is provided to determine compliance with the dissolution requirements where stated in the individual monograph for dosage forms administered orally. In this general chapter, a dosage unit is defined as 1 tablet or 1 capsule or the amount specified. Of the types of apparatus designs described herein, use the one specified in the individual monograph. Where the label states that an article is enteric coated and a dissolution or disintegration test does not specifically state that it is to be applied to delayed-release articles and is included in the individual monograph, the procedure and interpretation given for Delayed-Release Dosage Forms are applied, unless otherwise specified in the individual monograph. 本测试用于检测药品口服制剂的溶出度是否符合各论中的规定。本章中，除另有规定外，单位制剂定义为1片或1粒胶囊。对于本章中所述多种仪器，使用各论中规定的种类。除各论中另有规定外，如果检品是肠溶衣片且各论中的溶出度或崩解时限检查项下没有特别指出适用迟释剂的，使用本章中适用于迟释剂的流程和解释。 FOR DOSAGE FORMS CONTAINING OR COATED WITH GELATIN涂有或包含明胶的剂型 If the dosage form containing gelatin does not meet the criteria in the appropriate Acceptance Table (see Interpretation, Immediate-Release Dosage Forms, Extended-Release Dosage Forms, or Delayed-Release Dosage Forms) because of evidence of the presence of cross-linking, the dissolution procedure should be repeated with the addition of enzymes to the medium, as described below, and the dissolution results should be evaluated starting at the first stage of the appropriate Acceptance Table. It is not necessary to continue testing through the last stage (up to 24 units) when criteria are not met during the first stage testing, and evidence of cross-linking is observed. 如果剂型中含有明胶，其不符合验收表中的标准（见判断，速释制剂，延释制剂，缓释制剂），因为存在明胶交联结合作用，它的溶解过程与外加的媒介酶是重复的，见下面的描述，并且溶解结果可以通过适当的验收表的开始的第一阶段标准进行评估。如果溶出结果不满足第一阶段的测试标准，那么就没有必要继续测试到最后阶段，并且也证明了明胶交联结合作用的存在。

美国药典(USP)规定的色谱柱编号

美国药典(USP)规定的色谱柱编号 L1和L8是美国药典(USP)规定的色谱柱编号，其实就是ODS柱和NH2柱。下面是USP规定的编号所对应的色谱柱类型。 L1：十八烷基键合多孔硅胶或无机氧化物微粒固定相，简称ODS柱 L2：30～50m m表面多孔薄壳型键合十八烷基固定相，简称C18柱 L3：多孔硅胶微粒，即一般的硅胶柱 L4：30～50m m表面多孔薄壳型硅胶柱 L5：30～50m m表面多孔薄壳型氧化铝柱 L6：30～50m m实心微球表面包覆磺化碳氟聚合物，强阳离子交换柱 L7：全多孔硅胶微粒键合C8官能团固定相，简称C8柱 L8：全多孔硅胶微粒键合非交联NH2固定相，简称NH2柱 L9：强酸性阳离子交换基团键合全多孔不规则形硅胶固定相，即SCX柱 L10：多孔硅胶微球键合氰基固定相（CN），简称CN柱 L11：键合苯基多孔硅胶微球固定相，简称苯基柱 L12：无孔微球键合季胺功能团的强阴离子交换柱 L13：三乙基硅烷化学键合全多孔硅胶微球固定相（C1），简称C1柱 L14：10m m硅胶化学键合强碱性季铵盐阴离子交换固定相，简称SAX柱 L15：已基硅烷化学键合全多孔硅胶微球固定相，简称C6柱 L16：二甲基硅烷化学键合全多孔硅胶微粒固定相 C2柱 L17：氢型磺化交联苯乙烯-二乙烯基苯共聚物,强阳离子交换柱 L18：3～10m m全多孔硅胶化学键合胺基（NH2）和氰基（CN）柱 L19：钙型磺化交联苯乙烯－二乙烯基苯共聚物，强阳离子交换柱 L20：二羟基丙烷基化学键合多孔硅胶微球固定相（Diol），简称二醇基柱 L21：刚性苯乙烯－二乙烯基苯共聚物微球填料柱

美国药典USP31 71 无菌检查法中文版

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USP《671》美国药典-包装容器——性能检测译文

《671》包装容器——性能检测 本章规定了用来包装的塑料容器及其组件功能性质上的标准(药品、生物制剂、营养补充剂和医疗器械)，定义了保存、包装、存储和标签方面的凡例与要求。本文提供的试验用于确定塑料容器的透湿性和透光率。盛装胶囊和片剂的多单元容器章节适用于多单元容器。盛装胶囊和片剂的单位剂量容器章节适用于单位剂量容器。盛装胶囊和片剂的多单元容器(没有密封) 的章节适用于没有密封的聚乙烯和聚丙烯容器。盛装液体的多元和单元容器的章节适用于多元的和单元的容器。 一个容器想要提供避光保护或作为一个符合耐光要求的容器，由具有耐光的特殊性质的材料组成，包括任何涂层应用。一个无色透明或半透明的容器通过一个不透明的外壳包装变成耐光的(见凡例和要求 )，可免于对光的透射要求。在多单元容器和封盖与水泡的单位剂量容器由衬垫密封情况下，此处使用的术语“容器”指的是整个系统的组成。 盛装胶囊和片剂的多元容器 干燥剂——放置一些颗粒4—8目的无水氯化钙在一个浅的容器里，仔细剔除细粉，然后置于110°干燥，并放在干燥器中冷却。 试验过程——挑选12个类型和尺寸一致的容器，用不起毛的毛巾清洁密闭表面，并打开和关闭每个容器30次。坚决每次应用容器密闭一致。通过扭矩关闭螺旋盖容器，使气密性在附表规定的范围内。10个指定的测试容器添加干燥剂，如果容器容积大于等于20mL，每个填充13mm以内封闭；如果容器的容积小于20毫升，每个填充容器容量的三分之二。如果容器内部的深度超过63mm，惰性填料或垫片可以放置在底部来最小化容器和干燥剂的总重量；干燥剂层在这样一个容器中深度不低于5cm。添加干燥剂之后，立即按附表中规定的扭矩封闭螺旋帽容器。剩余的2个指定为对照容器，每个添加足够数量的玻璃珠，重量约等于每个测试容器的重量，并用附表中规定的扭矩封闭螺旋帽容器。记录各个容器的重量，如果容器的容积小于20毫升，精确到0.1毫克；如果容器容积为20毫升或以上但小于200毫升，精确到毫克；如果容器容积为200毫升及以上，精确到厘克（10毫克）；在相对湿度75±3%和温度23±2°的环境下存储。[注意——浓度为35g/100mL的氯化钠溶液放在干燥器底部的渗透系统来维持指定湿度。其他的方法可以用来维护这些条件。] 336±1小时（14天）后，用同样的办法记录每个容器的重

usp美国药典结构梳理

USP35-NF-30结构整理 vivi2010-10-02 USP总目录： 1 New Official Text修订文件 加快修订过程包括勘误表，临时修订声明（IRAS），修订公告。勘误表，临时修订声明，修订公告在USP网站上New Official Text部分刊出，勘误表，临时修订公告也会在PF上刊出2front matter前言 药典与处方集增补删减情况，审核人员，辅料收录情况 3凡例

药典， 1标题和修订 2 药典地位和法律认可 3标准复合性 4专论和通则 5 专论组成 6 检验规范和检验方法 7 测试结果 8 术语和定义 9 处方和配药 10 包装存储与标签 4通则 4.1章节列表 4.2一般检查和含量测定（章节编号小于1000）

检查和含量分析的一般要求 检查和含量分析的仪器， 微生物检查，生物检查和含量测定， 化学检查和含量测定， 物理检查和测定 4.3一般信息（章节号大于1000） 5食物补充剂通则 6试剂（试剂，指示剂，溶液等） 7参考表 性状描述和溶解性查询表（按字母顺序） 8食品补充剂各论（字母顺序） 9NF各论（辅料标准） 10 USP各论 11术语 附件：通则的章节中文目录（使用起来比较方便，直接找对应章节号即可）一、通用试验和检定 （1）试验和检定的总要求 1 注射剂 11 参比标准物 （2）试验和检定的装置 16 自动分析方法 21 测温仪 31 容量装置，如容量瓶、移液管、滴定管，各种规格的误差限度

41 砝码和天平 （3）微生物学试验 51 抗菌效力试验 55 生物指示剂：耐受性能试验 61 微生物限度试验 61 非灭菌制品的微生物检查：计数试验 62 非灭菌制品的特定菌检查，如大肠杆菌、金葡菌、沙门氏菌等 71 无菌试验 （4）生物学试验和检定 81 抗生素微生物检定 85 细菌内毒素试验 87 体外生物反应性试验：检查合成橡胶、塑料、高聚物对哺乳类细胞培养的影响 88 体内生物反应性试验：检查上述物质对小鼠、兔iv、ip或肌内植入的影响 91 泛酸钙检定 111 生物检定法的设计和分析 115 右泛醇检定 121 胰岛素检定 141 蛋白质——生物适应试验，用缺蛋白饲料大鼠，观察水解蛋白注射液和氨基酸混合物的作用 151 热原检查法 161 输血、输液器及类似医疗装置的内毒素、热原、无菌检查 171 维生素B12 活性检定 （5）化学试验和检定 A 鉴别试验 181 有机含氮碱的鉴别 191 一般鉴别试验 193 四环素类鉴别 197 分光光度法鉴别试验 201 薄层色谱鉴别试验 B 限量试验

USP美国药典 233元素杂质-检查法

á233? ELEMENTAL IMPURITIES—PROCEDURES INTRODUCTION This chapter describes two analytical procedures (Procedures 1 and 2) for the evaluation of the levels of the elemental impuri-ties. The chapter also describes criteria for acceptable alternative procedures. By means of validation studies, analysts will confirm that the analytical procedures described herein are suitable for use on specified material. Use of Alternative Procedures The chapter also describes criteria for acceptable alternative procedures. Alternative procedures that meet the validation re-quirements herein may be used in accordance with General Notices and Requirements 6.30, Alternative and Harmonized Meth-ods and Procedures . Information on the Requirements for Alternate Procedure Validation is provided later in this chapter.Speciation The determination of the oxidation state, organic complex, or combination is termed speciation . Analytical procedures for spe-ciation are not included in this chapter, but examples may be found elsewhere in USP–NF and in the literature. PROCEDURES ? C OMPENDIAL P ROCEDURES 1 AND 2 System standardization and suitability evaluation using applicable reference materials should be performed on the day of analysis. Procedure and detection technique:Procedure 1 can be used for elemental impurities generally amenable to detection by inductively coupled plasma–atomic (optical) emission spectroscopy (ICP–AES or ICP–OES). Procedure 2 can be used for ele-mental impurities generally amenable to detection by ICP–MS. Before initial use, the analyst should verify that the proce- dure is appropriate for the instrument and sample used (procedural verification) by meeting the alternative procedure vali-dation requirements below. Sample preparation:Forms of sample preparation include Neat , Direct aqueous solution , Direct organic solution , and Indi- rect solution . The selection of the appropriate sample preparation depends on the material under test and is the responsibil-ity of the analyst. When a sample preparation is not indicated in the monograph, an analyst may use any of the following appropriately validated preparation procedures. In cases where spiking of a material under test is necessary to provide an acceptable signal intensity, the blank should be spiked with the same Target elements , and where possible, using the same spiking solution. Standard solutions may contain multiple Target elements . [N OTE —All liquid samples should be weighed.]Neat:Used for liquids or alternative procedures that allow the examination of unsolvated samples. Direct aqueous solution:Used when the sample is soluble in an aqueous solvent. Direct organic solution:Used where the sample is soluble in an organic solvent. Indirect solution:Used when a material is not directly soluble in aqueous or organic solvents. Total metal extraction is the preferred sample preparation approach to obtain an Indirect solution . Digest the sample using the Closed vessel diges-tion procedure provided below or one similar to it. The sample preparation scheme should yield sufficient sample to allow quantification of each element at the limit specified in the corresponding monograph or chapter. Closed vessel digestion:This sample preparation procedure is designed for samples that must be digested in a Concen-trated acid using a closed vessel digestion apparatus. Closed vessel digestion minimizes the loss of volatile impurities. The choice of a Concentrated acid depends on the sample matrix. The use of any of the Concentrated acids may be appropri-ate, but each introduces inherent safety risks. Therefore, appropriate safety precautions should be used at all times. [N OTE —Weights and volumes provided may be adjusted to meet the requirements of the digestion apparatus used.] An example procedure that has been shown to have broad applicability is the following. Dehydrate and predigest 0.5 g of primary sample in 5 mL of freshly prepared Concentrated acid . Allow to sit loosely covered for 30 min in a fume hood.Add an additional 10 mL of Concentrated acid , and digest, using a closed vessel technique, until digestion or extraction is complete. Repeat, if necessary, by adding an additional 5 mL of Concentrated acid . [N OTE —Where closed vessel digestion is necessary, follow the manufacturer’s recommended procedures to ensure safe use.] Alternatively, leachate extraction may be appropriate with justification following scientifically validated metal disposition studies, which may include animal studies, speciation, or other means of studying disposition of the specific metal in the drug product. Reagents:All reagents used for the preparation of sample and standard solutions should be free of elemental impurities,in accordance with Plasma Spectrochemistry á730?. ? P ROCEDURE 1: ICP–OES Standardization solution 1: 1.5J of the Target element(s) in a Matched matrix Standardization solution 2:0.5J of the Target element(s) in a Matched matrix Sample stock solution:Proceed as directed in Sample preparation above. Allow the sample to cool, if necessary. For mer-cury determination, add an appropriate stabilizer. Sample solution:Dilute the Sample stock solution with an appropriate solvent to obtain a final concentration of the Target elements at NMT 1.5J . Blank: Matched matrix 298 á233? Elemental Impurities—Procedures / Chemical Tests USP 40

美国药典USP31(921)翻译版(上)

921WATER DETERMINATION水分测定 Many Pharmacopeial articles either are hydrates or contain water in adsorbed form. As a result, the determination of the water content is important in demonstrating compliance with the Pharmacopeial standards. Generally one of the methods given below is called for in the individual monograph, depending upon the nature of the article. In rare cases, a choice is allowed between two methods. When the article contains water of hydration, the Method I (Titrimetric), the Method II (Azeotropic), or the Method III (Gravimetric) is employed, as directed in the individual monograph, and the requirement is given under the heading Water. 很多药典物品要么是水合物，要么含有处于吸附状态的水。因此，测定水分含量对于证实与药典标准的符合性是很重要的。通常，在具体的各论中会根据该物品的性质，要求使用下面若干方法中的一个。偶尔，会允许在2个方法中任选一个。当该物品含有水合状态的水，按照具体各论中的规定，使用方法I（滴定测量法）、方法II（恒沸测量法）、或方法III（重量分析法），这个要求在标题水分项下给出。 The heading Loss on drying (see Loss on Drying 731) is used in those cases where the loss sustained on heating may be not entirely water. 在加热时的持续失重可能不全是水分的情况下，使用标题干燥失重（见干燥失重<731>）。 METHOD I (TITRIMETRIC) 方法I（滴定测量法） Determine the water by Method Ia, unless otherwise specified in the individual monograph. 除非具体各论中另有规定，使用方法Ia来测定水分。 Method Ia (Direct Titration) 方法Ia（直接滴定） Principle— The titrimetric determination of water is based upon the quantitative reaction of water with an anhydrous solution of sulfur dioxide and iodine in the presence of a buffer that reacts with hydrogen ions. 原理：水分的滴定法检测是基于水与二氧化硫的无水溶液以及存在于缓冲液中与氢离子反应的碘之间的定量反应。 In the original titrimetric solution, known as Karl Fischer Reagent, the sulfur dioxide and iodine are dissolved in pyridine and methanol. The test specimen may be titrated with the Reagent directly, or the analysis may be carried out by a residual titration procedure. The stoichiometry of the reaction

USP色谱柱解释

L1和L8是美国药典(USP)规定的色谱柱编号，其实就是C18柱和NH2柱。下面是对应的色谱柱类型。 L1：十八烷基键合多孔硅胶或无机氧化物微粒固定相，简称C18或ODS L2：30～50um表面多孔薄壳型键合C18(ODS)固定相 L3：多孔硅胶微粒即一般的硅胶柱 L4：30～50um表面多孔薄壳型硅胶 L5：30～50um表面多孔薄壳型氧化铝 L6：30～50um实心微球表面包覆磺化碳氟聚合物－强阳离子交换固定相 L7：全多孔硅胶微粒键合C8官能团固定相简称C8柱 L8：全多孔硅胶微粒键合非交联NH2固定相简称NH2柱 L9：强酸性阳离子交换基团键合全多孔不规则形硅胶固定相 L10：多孔硅胶微球键合氰基固定相（CN）简称CN柱 L11：键合苯基多孔硅胶微球固定相简称苯基柱 L12：无孔微球键合季胺功能团的强阴离子填料 L13：三乙基硅烷化学键合全多孔硅胶微球固定相（C1）简称C1柱 L14:10um硅胶化学键合强碱性季铵盐阴离子交换固定相简称SAX柱 L15：已基硅烷化学键合全多孔硅胶微球固定相简称C6柱 L16：二甲基硅烷化学键合全多孔硅胶微粒固定相 L17：氢型磺化交联苯乙烯-二乙烯基苯共聚物,强阳离子交换树脂 L18: 3～10um全多孔硅胶化学键合胺基（NH2）和氰基（CN） L19：钙型磺化交联苯乙烯－二乙烯基苯共聚物，强阳离子交换树脂 L20：二羟基丙烷基化学键合多孔硅胶微球固定相（Diol）简称二醇基柱 L21：刚性苯乙烯－二乙烯基苯共聚物微球 L22：带有磺酸基团的多孔苯乙烯阳离子交换树脂 L23：带有季胺基团的聚甲基丙烯酸甲酯或聚丙烯酸酯多孔离子交换树脂 L24：表面含有大量羟基的半刚性聚乙烯醇亲水凝胶 L25：聚甲基丙烯酸酯树脂交联羟基醚（表面含有残余羧基功能团）树脂。能分离分子量100～5000MW范围的水溶性中性、阳离子型及阴离子型聚合物（用聚氧乙烯测定）的固定相 L26：丁基硅烷化学键合全多孔硅胶微球固定相 L27：30～50um的全多孔硅胶微粒

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美国药典USP气相色谱柱对照表 L62 C30硅胶键合于完全多孔球状硅胶，粒径3~15μm。 G48 Highly polar, partially cross-linked cyanopolysiloxane. Rt-2560 G46 14% 氰丙基苯基- 86% 甲基聚硅氧烷 CB-1701MXT?-1701Rtx?-1701VF-1701ms OV-1701CBX-1701DB-1701DB-1701P G43 6% 氰丙基苯基- 94% 二甲基聚硅氧烷 MXT?-624DB-624MXT?-Volatiles CBX-1301 MXT?-1301OV-1301CB-624Rtx?-1301 VF-624ms/VF-1301ms Rtx?-624CB-1301CBX-624 G42 35% 苯基- 65% 二甲基乙烯聚硅氧烷 DB-35Rtx?-35MXT?-35CBX-35 HP-35DB-35MS G38 固定相G1 加减尾剂 MXT-1Rtx?-1MS Rtx?-1 G36 1% 乙烯基- 5% 苯基甲基聚硅氧烷 Rtx?-5MS Rtx?-5CBX-5MXT?-5 G35 聚乙二醇和硝基对苯二甲酸二乙二醇酯 DB-FFAP HP-FFAP CB-FFAP G32 20% Phenylmethyl-80% dimethylpolysiloxane. MXT?-20 G27 5% 苯基- 95% 甲基聚硅氧烷 CB-5XTI?-5Rtx?-5SIL MS VF-5ms Rtx?-5PONA HP-5MS HP-5DB-5MS SE-52DB-5SE-54 G25 聚乙二醇TPA（Carbowax 20M 对苯二酸） FFAP CBX-FFAP G19 25% 苯基- 25% 氰丙基甲基聚硅氧烷 OV-225Rtx?-225VF-23ms CBX-225 G17 75% 苯基- 25% 甲基聚硅氧烷 MXT?-65 G16 聚乙二醇（平均分子量15,000） DB-WAX CBX-Wax CB-WAX Stabilwax?PEG-20M Stabilwax?-DB Stabilwax?-DA MXT?-WAX

美国药典USP40-左氧氟沙星API

USP 40 Official Monographs / Levofloxacin 4831 Acceptance criteria: See Table 1. Sample solution: 1mg/mL of Levofloxacin in Mobile phase Chromatographic system Table 1(See Chromatography ?621?, System Suitability .)Relative Relative Acceptance Mode: LC Retention Response Criteria,Detector: UV 360 nm Name Time Factor NMT (%) Column: 4.6-mm × 25-cm; 5-μm packing L1Levodopa related Column temperature: 45°compound A 0.90.830.1Flow rate: 0.8mL/min Injection size: 25μL Levodopa 1.0——System suitability Levodopa related Sample: Standard solution compound B 2.8 0.83 0.5 Suitability requirements 5,6-Dihydroxy-in-Tailing factor: 0.5–1.5 dole-2-carboxylic Relative standard deviation: NMT 1.0%acid 6.0 2.5 0.1Analysis 0.1Samples: Standard solution and Sample solution individual Calculate the percentage of levofloxacin (C 18H 20FN 3O 4)— 0.3 total in the portion of Levofloxacin taken: Unknown impurities 1.0unknown Total impurities — — 1.1 Result = (r U /r S ) × (C S /C U ) × 100 r U = peak response of levofloxacin from the Sample ADDITIONAL REQUIREMENTS solution ?P ACKAGING AND S TORAGE : Preserve in tight, light-resistant r S = peak response of levofloxacin from the containers, in a dry place, and prevent exposure to ex-Standard solution cessive heat. C S = concentration of USP Levofloxacin RS in the ?USP R EFERENCE S TANDARDS ?11?Standard solution (mg/mL) USP Levodopa RS C U = concentration of Levofloxacin in the Sample USP Levodopa Related Compound A RS solution (mg/mL) 3-(3,4,6-Trihydroxyphenyl)alanine.Acceptance criteria: 98.0%–102.0% on the anhydrous C 9H 11NO 5213.19 basis USP Levodopa Related Compound B RS 3-Methoxytyrosine.IMPURITIES C 10H 13NO 4211.22 ?R ESIDUE ON I GNITION ?281?: NMT 0.2%. Use a platinum crucible. Delete the following: Levofloxacin ??H EAVY M ETALS , Method II ?231?: NMT 10ppm ?(Official 1-Jan-2018) ?O RGANIC I MPURITIES , P ROCEDURE 1 [N OTE —Procedure 1 is recommended if levofloxacin N -ox-ide is a potential organic impurity. Procedure 2 and Pro-cedure 3 are recommended if levofloxacin related com-pound B is a potential organic impurity.] Solution A, Mobile phase, Sample solution, and Chro-matographic system: Proceed as directed in the C 18H 20FN 3O 4·1/2H 2O 370.38Assay . 7H -Pyrido[1,2,3-de ]-1,4-benzoxazine-6-carboxylic acid, System suitability solution: 1mg/mL of USP Levoflox-9-fluoro-2,3-dihydro-3-methyl-10-(4-methyl-1-piperazinyl)-acin RS in Mobile phase 7-oxo-hydrate (2:1), (S )-; Sensitivity solution: 0.3μg/mL of USP Levofloxacin RS (?)-(S )-9-Fluoro-2,3-dihydro-3-methyl-10-(4-methyl-1-piper-in Mobile phase azinyl)-7-oxo-7H -pyrido[1,2,3-de ]-1,4-benzoxazine-6-car-System suitability boxylic acid, hemihydrate [138199-71-0].Samples: System suitability solution and Sensitivity Anhydrous [100986-85-41]. solution Suitability requirements DEFINITION Relative standard deviation: NMT 1.0%, System suit-Levofloxacin contains NLT 98.0% and NMT 102.0% of ability solution C 18H 20FN 3O 4, calculated on the anhydrous basis.Signal-to-noise ratio: NLT 10, Sensitivity solution IDENTIFICATION Analysis ?A . I NFRARED A BSORPTION ?197K ? Sample: Sample solution ?B . The retention time of the major peak of the Sample Calculate the percentage of each individual impurity in solution corresponds to that of the Standard solution , as the portion of Levofloxacin taken: obtained in the Assay.Result = (r U /r S ) × (1/F ) × 100 ASSAY ?P ROCEDURE r U = peak response of each impurity Buffer: 8.5g/L of ammonium acetate, 1.25g/L of cu-r S = peak response of levofloxacin pric sulfate, pentahydrate, and 1.3g/L of L -isoleucine in F = relative response factor (see Table 1)water Acceptance criteria: See Table 1. Mobile phase: Methanol and Buffer (3:7) Standard solution: 1mg/mL of USP Levofloxacin RS in Mobile phase USP Monographs