Avobenzone USP

2566Aurothioglucose / Official Monographs USP 36USP Reference standards 〈11〉—USP Avobenzone RS Aurothioglucose Injectable SuspensionIdentification—A: Infrared Absorption 〈197K 〉.» Aurothioglucose Injectable Suspension is a ster-B: Ultraviolet Absorption 〈197U 〉—ile suspension of Aurothioglucose in a suitable Solution: 5µg per mL.vegetable oil. It contains not less than 90.0per-Medium: alcohol.cent and not more than 110.0percent of the la-Absorptivities at 360 nm do not differ by more than beled amount of C 6H 11AuO 5S. It may contain 3.0%.suitable thickening agents.Melting range, Class I 〈741〉: between 81° and 86°.Loss on drying 〈731〉—Dry it in vacuum at 70° for 4hours:Packaging and storage—Preserve in single-dose or in it loses not more than 0.5% of its weight.multiple-dose containers, preferably of Type I glass. Protect Chromatographic purity—from light.Test solution—Proceed as directed for Assay preparation in USP Reference standards 〈11〉—the Assay .USP Aurothioglucose RSChromatographic system (see Chromatography 〈621〉)—Identification—Transfer a volume of Injectable Suspension,Proceed as directed in the Assay .equivalent to about 200mg of aurothioglucose, to a centri-fuge separator containing 20mL of ethyl acetate and 50mL Procedure—Inject a volume (about 1µL) of Test solution of water. Shake the mixture thoroughly, and centrifuge until into the chromatograph, record the chromatogram, and the liquid phases have been clearly separated. Withdraw the measure the peak responses. Calculate the percentage of lower, aqueous phase, and filter, discarding the first 10mL each impurity in the portion of Avobenzone taken by the of the filtrate. Collect the filtrate in a glass-stoppered vessel,formula:and proceed as directed in Identification test A under100(r I /r S )Aurothioglucose , beginning with “apply 10µL of this solu-tion.”in which r I is the response of each individual peak, other Bacterial endotoxins 〈85〉—It contains not more than than the avobenzone peak, in the chromatogram of the Test 7.14 USP Endotoxin Units per mg of aurothioglucose.solution; and r S is the sum of the responses of all of the Sterility 〈71〉—It meets the requirements.peaks in the chromatogram of the Test solution: not more Other requirements—It meets the requirements under In-than 3.0% of any individual impurity is found, and the sum jections 〈1〉.of all of the impurities is not more than 4.5%.Assay—Transfer with a pipet, calibrated to contain rather Assay—than to deliver, an accurately measured volume of Injectable Standard preparation—Dilute an accurately measured Suspension, equivalent to about 200mg of aurothioglucose,quantity of USP Avobenzone RS in acetone, and dilute to a beaker containing 400mL of acetone. Wash the pipet quantitatively, and stepwise if necessary, with acetone to into the beaker with a small quantity of acetone, mix, allow obtain a solution having a known concentration of about the solids to settle, and decant the supernatant through a 50mg per mL.filter. Wash the solids with another 400-mL portion of ace-Assay preparation—Transfer about 500mg oftone, and repeat the decantation. Transfer the solids to the Avobenzone, accurately weighed, to a 10-mL volumetric filter with the aid of acetone, then transfer the filter and its flask, dilute with acetone to volume, and mix.contents to a short-necked, 300-mL Kjeldahl flask, add 5mL Chromatographic system (see Chromatography 〈621〉)—The of water, and proceed as directed in the Assay under Gold gas chromatograph is equipped with a flame-ionization de-Sodium Thiomalate , beginning with “add 20mL of nitric tector and a 0.32-mm × 25-m fused silica capillary column acid.” The weight of gold so obtained, multiplied by 1.991,coated with phase G1. The column temperature is main-represents the weight of C 6H 11AuO 5S in the portion of In-tained at about 200° until the time of injection, then in-jectable Suspension taken.creased at a rate of 4° per minute to 280°. The injection port temperature is maintained at 200°, and the detector temperature is maintained at about 280°. Helium is used as the carrier gas. The split ratio is 50:1. Chromatograph the Standard preparation, and record the peak responses as di-Avobenzonerected for Procedure: the resolution, R, between avobenzone and any adjacent peak is not less than 1.0; and the relative standard deviation for replicate injections is not more than 2.0%.Procedure—Separately inject equal volumes (about 1µL)of the Standard preparation and the Assay preparation into the chromatograph, record the chromatograms, and meas-C 20H 22O 3310.39ure the responses for the major peaks. Calculate the quan-1,3-Propanedione, 1-[4-(1,1-dimethylethyl)phenyl]-tity, in mg, of C 20H 22O 3 in the portion of Avobenzone taken 3-(4-methoxyphenyl)-.by the formula:1-(p -tert -Butylphenyl)-3-(p -methoxyphenyl)-1,3-propane-dione [70356-09-1].10C (r U /r S )» Avobenzone contains not less than 95.0per-in which C is the concentration, in mg per mL, of USP Avobenzone RS in the Standard preparation; and r U and r S cent and not more than 105.0percent of are the peak responses obtained from the Assay preparation C 20H 22O 3, calculated on the dried basis.and the Standard preparation, respectively.Packaging and storage—Preserve in tight, light-resistant containers.USP 36Official Monographs / Azaperone2567Azaperone Azaperone Injection» Azaperone Injection is a sterile solution ofAzaperone in Water for Injection, prepared withthe aid of Tartaric Acid. It may contain a suitableC19H22FN3O327.40preservative and a stabilizing agent. It contains1-Butanone, 1-(4-fluorophenyl)-4-[4-(2-pyridinyl)-not less than 90.0percent and not more than1-piperazinyl]-.110.0percent of the labeled amount of4′-Fluoro-4-[4-(2-pyridyl)-1-piperazinyl]butyrophenoneC19H22FN3O.[1649-18-9].Packaging and storage—Preserve in single-dose or in» Azaperone contains not less than 98.0percentmultiple-dose containers, preferably of Type I glass, pro-and not more than 102.0percent of C19H22FN3O,tected from light.calculated on the dried basis.Labeling—Label it to indicate that it is for veterinary useonly.Packaging and storage—Preserve in well-closed contain-ers, protected from light. Store at room P Reference standards 〈11〉—USP Azaperone RSLabeling—Label it to indicate that it is for veterinary useonly.Identification—The chromatogram of the Assay prepara-tion obtained as directed in the Assay exhibits a major peak USP Reference standards 〈11〉—for azaperone, the retention time of which corresponds to USP Azaperone RSthat exhibited in the chromatogram of the Standard prepa-Identification, Infrared Absorption 〈197K〉: previously dried.ration, obtained as directed in the Assay.Melting range 〈741〉: between 92° and 95°.pH 〈791〉: between 4.0 and 5.6.Loss on drying 〈731〉—Dry it in vacuum at 60° for 4hours:Other requirements—It meets the requirements under In-it loses not more than 0.5% of its weight.jections 〈1〉.Residue on ignition 〈281〉: not more than 0.1%.Assay—Chromatographic purity—Dissolve an accurately Mobile phase—Prepare a filtered and degassed mixture weighed quantity of USP Azaperone RS in a mixture of ace-containing 6 volumes of acetonitrile and 4 volumes of 0.01 tone and methylene chloride (5:1) to obtain a solution hav-M dibasic potassium phosphate, and adjust by the addition ing a concentration of 0.50mg per mL (Standard solution of dilute phosphoric acid (1 in 10) to a pH of 7.8 ± 0.1. A). Quantitatively dilute a volume of Standard solution A Make adjustments if necessary (see System Suitability under with the same solvent mixture to obtain a solution having a Chromatography 〈621〉).concentration of 0.25mg per mL (Standard solution B). Pre-Internal standard solution—Prepare a solution of benzo-pare a test solution by dissolving an accurately weighedphenone in methanol containing about 0.5mg per mL. quantity of Azaperone in a mixture of acetone and methyl-ene chloride (5:1) to obtain a solution containing 50mg per Standard preparation—Dissolve an accurately weighed mL. Separately apply 1µL each of Standard solution A, Stan-quantity of USP Azaperone RS in methanol, and dilute quan-dard solution B, and the test solution to a thin-layer chro-titatively with methanol to obtain a solution having a known matographic plate (see Chromatography 〈621〉) coated with concentration of about 0.5mg per mL. Combine 2.5mL of a 0.2-mm layer of chromatographic silica gel mixture with this solution with 2.5mL of Internal standard solution, dilute chemically bonded amino groups, and allow the spots to quantitatively with methanol to 10.0mL, and mix.dry. Develop the chromatograms in a solvent system con-Assay preparation—Dilute an accurately measured volume sisting of a mixture of cyclohexane, acetone, and methanol of Injection quantitatively with methanol to obtain a solu-(65:30:5) until the solvent front has moved about three-tion containing about 0.5mg of azaperone per mL. Com-fourths of the length of the plate. Remove the plate from bine 2.5mL of this solution with 2.5mL of Internal standard the chromatographic chamber, and allow the plate to air-solution, dilute quantitatively with methanol to 10.0mL, and dry. Examine the plate under short-wavelength UV light,mix.and compare the intensities of any secondary spots, other Chromatographic system (see Chromatography 〈621〉)—The than any spot at the origin, observed in the chromatogram liquid chromatograph is equipped with 243-nm detectorof the test solution with those of the principal spots in the and a 4.6-mm × 25-cm column that contains packing L1. chromatograms of Standard solution A and Standard solution The flow rate is about 2mL per minute. Chromatograph the B: the sum of the intensities of the secondary spots obtained Standard preparation, and record the peak responses as di-from the test solution corresponds to not more than the rected for Procedure: the resolution, R, between the azaper-intensity of the principal spot in the chromatogram of Stan-one and internal standard peaks is not less than 2.7; and dard solution A (1.0%).the relative standard deviation for replicate injections is not Assay—Dissolve about 120mg of Azaperone, accurately more than 2.0%.weighed, in 50mL of a mixture of methyl ethyl ketone and Procedure—Separately inject equal volumes (about 10µL) glacial acetic acid (7:1). Add 3drops of p-naphtholbenzein of the Standard preparation and the Assay preparation into TS, and titrate with 0.1 N perchloric acid VS. Perform a the chromatograph, record the chromatograms, and meas-blank determination, and make any necessary correction.ure the responses for the major peaks. Calculate the quan-Each mL of 0.1 N perchloric acid is equivalent to 16.37mg tity, in mg, of azaperone (C19H22FN3O) in each mL of theof C19H22FN3O.Injection taken by the formula:(C)(L/D)(R U/R S)in which C is the concentration, in mg per mL, of USPAzaperone RS in the Standard preparation; L is the labeledquantity, in mg, of azaperone in each mL of the Injection; Dis the concentration, in mg per mL, of azaperone in theAssay preparation, based on the volume of Injection taken。