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Standard preparation, and record the peak responses as di- Test solution—Transfer an accurately weighed portion of
rected for Procedure: the column efficiency is not less than the contents of 20 opened Capsules, equivalent to about
1500 theoretical plates; the tailing factor is not more than 250 mg of acebutolol, to a 100-mL volumetric flask, add
2.5; and the relative standard deviation for replicate injec- about 25 mL of methanol, and shake by mechanical means
tions is not more than 2.0%. for about 15 minutes. Dilute with Diluent to volume, and
Procedure—Separately inject equal volumes (about 10 µL) mix. Centrifuge a portion of this solution, and transfer
of the Standard preparation and the Assay preparation into 10.0 mL of the clear supernatant to a 100-mL volumetric
the chromatograph, record the chromatograms, and meas- flask. Dilute with Diluent to volume, and mix.
ure the responses for the major peaks. Calculate the quan- Chromatographic system (see Chromatography 〈621〉)—The
tity, in mg, of C18H28N2O4 · HCl in the portion of Acebutolol liquid chromatograph is equipped with a 240-nm detector
Hydrochloride taken by the formula: and a 3.9-mm × 15-cm column that contains 4-µm packing
L1. The flow rate is about 1 mL per minute. Chromatograph
250C(rU / rS) the Standard solution, and record the peak responses as di-
rected for Procedure: the relative standard deviation for repli-
in which C is the concentration, in mg per mL, of USP cate injections is not more than 6.0%.
Acebutolol Hydrochloride RS in the Standard preparation; Procedure—Separately inject equal volumes (about 35 µL)
and rU and rS are the acebutolol peak responses obtained of the Standard solution, Test solution, and Diluent into the
from the Assay preparation and the Standard preparation, re- chromatograph, record the chromatograms for about two
spectively. times the retention time of acebutolol, and measure the re-
sponses for all the peaks, disregarding any peaks corre-
sponding to those obtained from the Diluent. Calculate the
percentage of each impurity eluting prior to the acebutolol
peak in the portion of Capsules taken by the formula:
Acebutolol Hydrochloride Capsules
.
(336.44/372.89)(0.4C)(ri / rS)
» Acebutolol Hydrochloride Capsules contain the in which 336.44 and 372.89 are the molecular weights of
equivalent of not less than 90.0 percent and not acebutolol and acebutolol hydrochloride, respectively; C is
more than 110.0 percent of the labeled amount the concentration, in µg per mL, of USP Acebutolol Hydro-
of acebutolol (C18H28N2O4). chloride RS in the Standard solution; ri is the peak response
of any individual impurity obtained from the Test solution;
Packaging and storage—Preserve in tight containers, and and rS is the peak response of acebutolol obtained from the
store at controlled room temperature. Standard solution: not more than 0.5% of any individual im-
USP Reference standards 〈11〉— purity is found.
USP Acebutolol Hydrochloride RS TEST 2—
Identification—The retention time of the major peak in Buffer solution—Prepare as directed in the Assay.
the chromatogram of the Assay preparation corresponds to Mobile phase—Prepare a filtered and degassed mixture of
USP Monographs
that in the chromatogram of the Standard preparation, as Buffer solution and methanol (50:50). Make adjustments if
obtained in the Assay. necessary (see System Suitability under Chromatography
Dissolution 〈711〉— 〈621〉).
Medium: water; 900 mL. Standard solution—Transfer about 30 mg of USP
Apparatus 2: 50 rpm. Acebutolol Hydrochloride RS, accurately weighed, to a
Time: 30 minutes. 50-mL volumetric flask. Add about 12 mL of methanol, swirl
to dissolve, dilute with Mobile phase to volume, and mix.
Procedure—Determine the amount of C18H28N2O4 dis- Dilute an accurately measured volume of this stock solution
solved by employing UV absorption at the wavelength of quantitatively, and stepwise if necessary, with Mobile phase
maximum absorbance at about 232 nm on filtered portions to obtain a solution having a known concentration of about
of the solution under test in comparison with a Standard 1.4 µg of USP Acebutolol Hydrochloride RS per mL.
solution having a known concentration of USP Acebutolol
Hydrochloride RS in the same Medium. Test solution—Transfer an accurately weighed portion of
the contents of 20 opened Capsules, equivalent to about
Tolerances—Not less than 80% (Q) of the labeled amount 250 mg of acebutolol, to a 100-mL volumetric flask, add
of acebutolol (C18H28N2O4) is dissolved in 30 minutes. about 25 mL of methanol, and shake by mechanical means
Uniformity of dosage units 〈905〉: meet the require- for about 15 minutes. Dilute with Mobile phase to volume,
ments. and mix. Centrifuge a portion of this solution, and transfer
Chromatographic purity— 10.0 mL of the clear supernatant to a 100-mL volumetric
TEST 1— flask. Dilute with Mobile phase to volume, and mix.
Buffer solution—Prepare as directed in the Assay. Chromatographic system (see Chromatography 〈621〉)—The
liquid chromatograph is equipped with a 240-nm detector
Mobile phase—Prepare a filtered and degassed mixture of and a 3.9-mm × 15-cm column that contains 4-µm packing
Buffer solution and methanol (56:44). Make adjustments if L1. The flow rate is about 1 mL per minute. Chromatograph
necessary (see System Suitability under Chromatography the Standard solution, and record the peak responses as di-
〈621〉). rected for Procedure: the relative standard deviation for repli-
Diluent—Prepare a mixture of Buffer solution and metha- cate injections is not more than 6.0%.
nol (50:50). Procedure—Separately inject equal volumes (about 70 µL)
Standard solution—Transfer about 30 mg of USP of the Standard solution, Test solution, and Mobile phase into
Acebutolol Hydrochloride RS, accurately weighed, to a the chromatograph, record the chromatograms for about
50-mL volumetric flask. Add about 12 mL of methanol, swirl three times the retention time of acebutolol, and measure
to dissolve, dilute with Diluent to volume, and mix. Dilute the responses for all the peaks, disregarding any peaks cor-
an accurately measured volume of this solution quantita- responding to those obtained from the Mobile phase. Calcu-
tively, and stepwise if necessary, with Diluent to obtain a late the percentage of each impurity eluting after the
solution having a known concentration of about 1.4 µg of
USP Acebutolol Hydrochloride RS per mL.
in which 336.44 and 372.89 are the molecular weights of rU = peak area response from the Sample solution
acebutolol and acebutolol hydrochloride, respectively; C is rS = peak area response from the Standard solution
the concentration, in mg per mL, of USP Acebutolol Hydro- CS = concentration of USP Acepromazine Maleate
chloride RS in the Standard preparation; and rU and rS are RS in the Standard solution (mg/mL)
the acebutolol peak responses obtained from the Assay prep- CU = concentration of the Sample solution (mg/mL)
aration and the Standard preparation, respectively. Acceptance criteria: 98.0%–101.0% on the anhydrous
basis
IMPURITIES
• RESIDUE ON IGNITION 〈281〉: NMT 0.2%
• ORGANIC IMPURITIES
.
Acepromazine Maleate Conduct this test without exposure to daylight, and with
the minimum necessary exposure to artificial light.
Diluent: Methanol and diethylamine (19:1)
Sample solution: 20.0 mg/mL of Acepromazine
Maleate in Diluent
Standard solution: 0.1 mg/mL of Acepromazine
Maleate in Diluent from the Sample solution