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Efavirez Tablets.
This monograph has been posted on the USP Pending Monographs Web page for review and public
comment for more than 90 days. A comment was received to Indentification test A from 250-300 nm
to 200-300 nm. The comment was incorporated and the MD-AA Expert Committe has approved the
monograph as an Authorized USP Pending Monograph.
The HPLC procedures in the assay and in test for organic impurities are based on analyses performed
with the hypersll efavirez peak is about 3.3 min for the assay and 10.3 min for the test for organic
impuruties.
(MD-AA: L. Santos, B. Davani. BPC: M. Marques.)
Definition
Efavirenz tablets contain NLT 92.0% and NMT 110.0 % of the labeled amount of efavirenz
(C14H9ClF3NO2)
Identification
-A. Ultraviolet Absorption <197U>
Wavelenght range: 200-300 nm
Medium: Proceed as directed in the test for Dissolution.
Sample solution: 16.8 g/mL of efavirenz in medium
-B. The retention time of the efavirenz peak of sample solution B corresponds to that of standard
solution B, as obtained in the test for organic impurities.
Assay
- Procedure
Buffer: 8.6 mg/mL of ammonium dihydrogen phosphate in water. Adjust with phosphoric acid to a PH
of 3.00 0.05 . Pass the solution through a suitable 0.45-m filter.
Mobile phase: acetonitrile and Buffer (3:2)
System suitability solution: 120 g/mL of USP Efavirenz RS and 1.8 g/mL of USP Efavirenz Related
Compound A RS in methanol.
Standard solution: 0.12 mg/mL of USP Efavirenz RS in methanol. Pass the solution through a suitable
0.45-m filter.
Sample stock solution: transfer an equvalent to 3000 mg of efavirenz (NLT 5 Tablets) to a 500-mL
volumetric flask, add 400 mL of metahanol, shake, and sonicate until the tablets have completely
disintegrated. Sonicate for another 20 min with intermittent swirling. Allow the solution to cool to
room temperature, and dilute with methanol to volume. Centrifuge an aliquot for 10 min at 500 rpm,
and use the filtrate.
Sample solution: 0.12 mg/mL of efavirenz from the sample stock solution in methanol. Pass the
solution through a suitable 0.45-m filter.
Chromatographic system
(see chromatography <621>, system suitability.)
Mode
: LC
Detector : UV 252 nm
Column : 4.6-mm 15-cm; 5-m packing L1
Flow rate : 1.5 mL/min
Injection size : 20 L
Column temperature
: 302
System suitability

Samples : system suitability solution and standard solution [Note-The realtive retention times are
listed in Impurity Ta-bale 1.]
Suitability requirements
Resolution: NLT 2 between efavirenz related compound A, System suitability solution
Column efficiency: NLT 3000 theoretical plates for efavirenz, System suitability solution
Talling factor: NMT 2.0 for efavirenz, system suitability solution
Related standard deviation: NMT 2.0 %, standard solution
Analysis
Samples: Standard solution and sample solution calculate the percentage of C 14H9ClF3NO2 in the
portion of Tablets taken:
Result = (rs/rs) (Cs/Cs) 100
Ru= peak response of efavirenz in the sample solution
Rs= peak response of efavirenz in the standard solution
Cs= concentration of USP Efavirenz RS in the standard solution (mg/mL)
Cu= nominal concentration of efavirenz in the sample solution (mg/mL)
Acceptance criteria: 92.0 %-110.0%
Performance tests
-Dissolution (711)
Medium: 2 % sodium lauryl sulfate in water; 900mL, degassed
Apparatus 2: 50 rpm
Time : 30 min
Standard solution : Transfer about 67 mg, accurately weight, of USP efavirenz RS to a 200mL volumetric flask, dissolve in 20 mL of methanol, and dilute with medium to volume.
Transfer 5.0 mL of this solution to a 100-mL volumetric flask, and dilute with medium to
volume.
Sample solution: pass a portion of the solution under test through a suitable 0.45-m filter .
Transfer 5.0 mL of the filtrate to a 200-mL volumetric flask, and dilute with medium to volume.
Spectrometric conditions
Mode: UV absorption apectroscopy
Analytical wavelenght: UV 248 nm
Cell lenght: 1 cm
Blank: medium
Calculate the percentage of C14H9ClF3NO2 in the portion of
Tablets taken :
Result = (Au/As) (Cs/L) V D 100
Au = absorbance of efavirenz from the sample solution
As = absorbance of efavirenz from the standard solution
Cs = concentration of USP efavirenz RS in the standard solution (mg/mL)
L = label claim (mg/tablet)
V = volume of medium, 900 mL
D = dilution factor of solution under test
Tolerances : NLT 80% (Q) of the labeled amount of efavirenz is dissolved.
Uniformity of dosage Units (905): Meet the requirements
Impurities
Organic Impurities
-procedure
Buffer: proceed as directed in the assay.

Solution A: Acetonitrile and Buffer (1:1)

Solution B: Acetonitrile and buffer (3:1)
Mobile phase: see the gradient table below
Time (min)
0
15
25
35
37
45

Solution A (%)
100
100
0
0
100
100

Solution B (%)
0
0
100
100
0
0

System suitability solution: 1mg/mL of USP Efavirenz RS and 2 g/mL of USP efavirenz related
compound A RS in methanol.

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Tablet Efavirez.
Monograf ini telah diposting pada halaman Web USP sebelumnya
Monograf untuk review dan komentar publik selama lebih dari 90 hari.
Sebuah komentar diterima untuk Identifikasi tes A 250-300 nm untuk 200300 nm. Komentar didirikan dan MD-AA Ahli Komite telah menyetujui
monografi sebagai Authorized USP Tertunda Monografi.Prosedur HPLC di uji
dan di tes untuk kotoran organik didasarkan pada analisis yang dilakukan
dengan puncak hypersll efavirez adalah sekitar 3,3 menit untuk pengujian
dan 10.3 menit untuk tes untuk impuruties organik.(MD-AA: L. Santos, B.
Davani BPC:.. M. Marques)DefinisiTablet efavirenz mengandung NLT 92.0%
dan
NMT
110,0%
dari
jumlah
berlabel
efavirenz
(C14H9ClF3NO2)Identifikasi-A.
Ultraviolet
Penyerapan
<197U>Kisaran
panjang gelombang: 200-300 nmSedang: Lanjutkan seperti diarahkan dalam
tes untuk Pembubaran.Contoh solusi: 16,8 mg / mL efavirenz dalam mediumB. Waktu retensi puncak efavirenz larutan sampel B sesuai dengan yang
larutan standar B, seperti yang diperoleh dalam tes untuk kotoran
organik.Pengujian kadar logam- ProsedurBuffer: 8,6 mg / mL amonium
dihidrogen fosfat dalam air. Sesuaikan dengan asam fosfat ke PH 3,00
0,05. Lulus solusi melalui filter 0,45-um cocok.Ponsel fase: asetonitril
dan Buffer (3: 2)Kesesuaian sistem solusi: 120 ug / mL USP Efavirenz RS
dan 1,8 mg / mL USP Efavirenz terkait Senyawa A RS dalam metanol.Larutan
standar: 0,12 mg / mL USP Efavirenz RS dalam metanol. Lulus solusi
melalui filter 0,45-um cocok.Contoh larutan stok: mentransfer equvalent
3000 mg efavirenz (NLT 5 Tablet) ke labu ukur 500 mL, tambahkan 400 ml
metahanol, goyang, dan sonicate sampai tablet memiliki sepenuhnya
hancur. Sonicate selama 20 menit dengan berputar-putar berselang.
Biarkan larutan dingin sampai suhu kamar, dan encerkan dengan metanol
untuk volume. Centrifuge sebuah aliquot selama 10 menit pada 500 rpm,
dan menggunakan filtrat.Larutan sampel: 0,12 mg / mL efavirenz dari
larutan stok sampel dalam metanol. Lulus solusi melalui filter 0,45-um
cocok.Sistem
kromatografi(Lihat
kromatografi
<621>,
kesesuaian
sistem.)Mode: LCDetektor: UV 252 nmKolom: 4.6-mm 15 cm; 5-um kemasan
L1Laju alir: 1,5 mL / menitUkuran Injection: 20 uLSuhu kolom: 30 2

Kesesuaian sistemSampel: solusi sistem kesesuaian dan larutan standar

[Catatan-Retensi realtive kali tercantum dalam kenajisan Ta-bale
1.]Persyaratan kesesuaianResolusi: NLT 2 antara efavirenz terkait
senyawa A, solusi Sistem kesesuaianEfisiensi kolom: NLT 3000 piring
teoritis untuk efavirenz, solusi Sistem kesesuaianFaktor talling: NMT
2.0 untuk efavirenz, solusi sistem kesesuaianTerkait standar deviasi:
NMT 2,0%, larutan standarAnalisaSampel: Standard solusi dan larutan
sampel menghitung persentase
C14H9ClF3NO2 dalam
porsi
Tablet
diambil:Hasil = (rs / rs) (Cs / Cs) 100Ru = respon puncak efavirenz
dalam larutan sampelRs = respon puncak efavirenz dalam larutan standarCs
= konsentrasi USP Efavirenz RS dalam larutan standar (mg / mL)Cu =
konsentrasi nominal efavirenz dalam larutan sampel (mg / mL)Kriteria
penerimaan: 92.0% -110,0%Tes kinerja-Dissolution (711)Sedang: 2% natrium
lauril sulfat dalam air; 900 ml, gasnyaAparat 2: 50 rpmWaktu: 30
menitStandar solusi: transfer sekitar 67 mg, akurat berat, dari USP
efavirenz RS ke labu ukur 200 mL, larut dalam 20 ml metanol, dan
encerkan dengan media untuk volume. Mentransfer 5.0 mL larutan ini ke
labu ukur 100 mL, dan encerkan dengan media untuk volume.Larutan sampel:
lulus sebagian dari solusi yang diuji melalui filter 0,45-um cocok.
Mentransfer 5.0 mL filtrat ke dalam labu volumetrik 200 mL, dan encerkan
dengan media untuk volume.Kondisi spektrometriMode: UV apectroscopy
penyerapanAnalitis panjang gelombang: UV 248 nmSel panjang: 1 cmKosong:
sedangHitung persentase C14H9ClF3NO2 dalam porsi Tablet diambil:Hasil =
(Au / As) (Cs / L) V D 100Au = absorbansi dari efavirenz dari
larutan sampelSebagai = absorbansi dari efavirenz dari larutan standarCs
= konsentrasi USP efavirenz RS dalam larutan standar (mg / mL)L = label
klaim (mg / tablet)V = volume sedang, 900 mLD = faktor pengenceran
larutan yang diujiToleransi: NLT 80% (Q) dari jumlah berlabel efavirenz
dibubarkan.Keseragaman
Unit
dosis
(905):
Memenuhi
persyaratanKotoranKotoran organik-prosedurBuffer: lanjutkan seperti
diarahkan dalam pengujian tersebut.Solusi: Asetonitril dan Buffer (1:
1)Solusi B: Asetonitril dan penyangga (3: 1)Fase gerak: lihat tabel di
bawah ini gradien