Orlistat CAS 96829-58-2 API Pondus Damnum Drug Puritas 98.0~ 101.5%

Orlistat
C29H53NO5 495.73
l-Leucine, N-formyl-, 1-[(3-hexyl-4-oxo-2-oxetanyl)methyl]dodecyl niensis [2S-[2(R*)]-;
N-Formyl-l-leucine, niensis cum (3S,4S) -3-hexyl-4-[(2S)-2-hydroxytridecyl]-2-oxetanone [96829-58-2].
DEFINITIO
Orlistat continet NLT 98.0% et NMT 101.5% C29H53NO5, calculi anhydroi, liberorum solvendi fundamentum.
IDENTIFICATIO
• A. Absorptio infrared <197M>
• B. Retentionis tempus maioris apicem solutionis Sample respondet solutioni vexilliferorum, prout habetur in Assay.
TEMPTATIO
• De modo procedendi
[Nota-Vite laguncularum plasticarum usum ad praeparationem seu continentiam cuiuslibet solutionis in hac analysi.]
Mobilis phase: Acetonitrile, Acidum phosphoricum, et aqua (860: 0.05: 140)
Solutio Standard: 0.5 mg/mL USP Orlistat RS in phase Mobilis.Injeci ftatim confecto , aut copia in 5 .
Sample solutio: 0.5 mg/mL Orlistat in phase Mobilis.Injeci ftatim confecto , aut copia in 5 .
Systema chromatographicum
(Vide Chromatographiam <621>, Ratio idoneitatis.)
Modus: LC
Detector: UV 195
Columna: 3.9-mm × 15-cm;4-µm stipare L1
Fluunt rate: 1.0 mL/min
Iniectio amplitudo: 20 µL
Ratio convenientia
Sample: Latin solution
Convenientia requisita
Relativum vexillum declinationis: NMT 2.0%
Analysis
Exempla: Standard solution et Sample solutionem
Recipis orlistat (C29H53NO5) in portione Orlistat capta;
Proventus = (rU/rS) (CS/CU) 100
rU = apicem responsio ex Sample solutione
rS = apicem responsio ex solutione Latin
CS = intentio USP Orlistat RS in solutione Standard (mg/mL)
CU = intentio Orlistat in solutione Sample (mg/mL)
Criteria acceptationis: 98.0% -101.5% in anhydroso, libero fundamento solvendo
IMPURITIES
Inorganic immunditias
• Residuum in Ignitione <281>: NMT 0.1%
• Metalla gravia, Methodus II <231>: 20 ppm .
Impurities organica
• De modo procedendi I: Finis Orlistat Related Compone A
Solutio Standard: 0.1 mg/mL of USP Orlistat Compone A RS in acetone
Sample solutio: 50 mg/mL of Orlistat in acetone
Systema chromatographicum
(Vide Chromatographia <621>, Thin-Layer Chromatographia.
Modus: TLC
Adsorbent: 0.25-mm iacuit chromatographico silicae gel mixtionis
Applicationem voluminis: 10 µL
Solvendo ratio explicandi: Toluene et acetas ethyla (4, 1).
Solutio deprehensio: Translatio 2.5 g acidi phosphomolybdici et 1 g sulfati cerrici in lagulam voluminis 100-mL, dissolve et methanolum ad volumen dilutum.
Analysis
Exempla: Standard solution et Sample solutionem
Aufer laminam, et eam penitus excoquatur.Sparge laminam aridam cum solutione detectionis, et pone laminam in clibano 120 pro 30 min.
Criteria acceptationis: Quaevis macula secundaria e solutione sample solutionis compositae orlistat affinis respondens, intensior non est quam macula respondet solutionis Standardi (0.2%).
• De modo procedendi II: Finis Orlistat Related Compone B
Solutio Standard: 0.025 mg/mL of USP Orlistat Compone B RS in methylene chloride
Sample solutio: 50 mg/mL Orlistat in methylene chloridi
Spicata solutionis specimen: 50 mg/mL de Orlistat in Standard solutione
Systema chromatographicum
(Vide Chromatographiam <621>, Ratio idoneitatis.)
Modus: GC
Detector: flamma ionization
Columna: 0.32-mm x 30-m silica fusis, 0.25-µm G27 periodo stationaria obducta.
Columna temperatus: Vide infra mensam programmatis temperatus.
Coepi Temperature () Temperature Ramp (/min) Final Temperature () Time at Final Temperature (min)
L 4 170 -
170 30 300 30
Temperature
Injector: 270
Detector: 280
Portitorem gas: Helium
Fluunt rate: 30 mL/min
Ratio split: 10:1
Magnitudo iniectio: 2 µL
Ratio convenientia
Sample: Latin solution
Convenientia requisita
Relativum vexillum declinationis: NMT 10.0%
Analysis
Exempla: Sample solutionem ac solutionem spicatam
Recipere recipis orlistat relatos compositi B in portione Orlistat sumpta;
Proventus = [rU/(rSP rU)] (CS/CT) 100
rU = apicem responsionis orlistat affinis compositi B ex solutione Sample
rSP = apicem responsum orlistat relatum compositum B ex solutione spicati spicati
CS = intentio USP Orlistat Composita B RS in Standard solutione (mg/mL)
CT = intentio Orlistat in Spiked solutionis specimen (mg/mL)
Receptae acceptationis: NMT 0.05% orlistat relatarum compositorum B invenitur.
• De modo procedendi 3
[Nota-Vite laguncularum plasticarum usum ad praeparationem seu continentiam cuiuslibet solutionis in hac analysi.]
Mobile phase, Standard solution, Sample solution: Para ut ordinatur in Perge.
Systema convenientiae solutionis: 10 µg/mL USP Orlistat RS, 0.1 µg/mL USP Orlistat Compositum C RS, et 0.25 µg/mL USP Orlistat Compositum D RS in tempore Mobili
Systema chromatographicum
(Vide Chromatographiam <621>, Ratio idoneitatis.)
Perge ad directum in Assay, nisi ad solutionem chromatographorum systematis idoneitatis.
Ratio convenientia
Sample: Ratio idoneitatis solutionis
Convenientia requisita
Rationis soni signum: NLT 3 pro compositis C orlistat affinibus et orlistat affinibus D iugis compositi.
Relativum vexillum digredior: NMT 10.0% ad orlistat apicem
Analysis
Exempla: Standard solution et Sample solutionem
Recipis cujusque immunditiae rationem in portione Orlistat sumta;
Proventus = (rU/rS) (CS/CU) (1/F) 100
rU = cacumen responsio ad singulas immunitates ex solutione Sample
rS = apicem responsionis USP Orlistat RS ex solutione Standard
CS = intentio USP Orlistat RS in solutione Standard (mg/mL)
CU = intentio Orlistat in solutione Sample (mg/mL)
F = responsio relativa facta in tabula immunditia 1
Re- gulae acceptationis: Vide Tabulam immunditiam 1 .
De immunitate Tabula 1
Nomen relativum Retentionis Time Relativi Response Factor Acceptationis Criteria, NMT (%)
Formylleucinea 0.10 4.0 0.2
Orlistat affinis compositi C 0.13 33 0.05
Orlistat anulum apertum epimerb 0.44 1.0 0.2
Orlistat affinis compositi D* 0.90 - Calculata in
De modo procedendi 4
Orlistat anulum apertum amidec* 0.90 - Calculatum in
De modo procedendi 4
Orlistat 1.00 - -
d-Leucine orlistatd 1.18 1.0 0.2
Impuratio individua unidentified - 1.0 0.1
* Coelutes in hac LC systemate, adhibito modo procedendi determinata.
a N-Formyl-l-leucine.
b (2S,3R,5S) -5-[(S)-2-Formylamino-4-methyl-pentanoyloxy] -2-hexyl-3-hydroxy-hexadecanoicum acidum.
c N-Formyl-l-leucine(S)-1-[(2S,3S)-2-hydroxy-3-[1-phenyl-R-ethylcarbomoyl]nonyl]-dodecyl niensis.
d N-Formyl-d-leucine(S)-1-[[(2S,3S)-3-hexyl-4-oxo-2-oxetanyl]methyl]dodecyl ester or enantiomer.
• De modo procedendi IV: Finis Orlistat Related Compone D
Mobile phase: Methanol and water (83:17)
Solutio aptabilitas systematis: 4 mg/mL of USP Orlistat RS et 2.4 µg/mL USP Orlistat Compositum D RS in acetonitrili affine, respectively.
Solutio Standard: 5.0 mg/mL of USP Orlistat RS in acetonitrili
Sample solutio: 5.0 mg/mL of Orlistat in acetonitrili
Systema chromatographicum
(Vide Chromatographia 621, Ratio Suitability).
Modus: LC
Detector: 205 nm
Columna: 4.0-mm × 25-cm;5-µm stipare L7
Fluunt rate: 0.6 mL/min
Iniectio amplitudo: 20 µL
Ratio convenientia
Sample: Ratio idoneitatis solutionis
Convenientia requisita
Rationis soni signum: NLT 3 pro orlistat affinis compositi D cacumen
Relativum vexillum digredior: NMT 10.0% ad orlistat apicem
Analysis
Exempla: Standard solution et Sample solutionem
Recipis cujusque immunditiae rationem in portione Orlistat sumta;
Proventus = (rU/rS) (CS/CU) (1/F) 100
rU = cacumen responsio ad singulas immunitates ex solutione Sample
rS = apicem responsio ad USP Orlistat RS ex solutione Standard
CS = intentio USP Orlistat RS in solutione Standard (μg/mL)
CU = intentio Orlistat in solutione Sample (μg/mL)
F = responsio relativa factor ut habetur in tabula immunditia 2
Re- gulae acceptationis: Vide Tabula immunditia II.
De immunitate Tabula 2
Nomen relativum Retentionis Time Relativi Response Factor Acceptationis Criteria, NMT (%)
Orlistat affinis compositi D 0.94 1.0 0.2
Orlistat 1.00 - -
Orlistat annulum apertum amidea 1.25 4.3 0.1
a N-Formyl-l-leucine(S)-1-[(2S,3S)-2-hydroxy-3-[1-phenyl-R-ethylcarbomoyl]nonyl]-dodecyl niensis.
• De modo procedendi V: Finis Orlistat Related Compone E
Quiddam: 0.4 N borata solutio, pH 10.2 . accommodata
Agens derivans: o-Phthaldehyde (OPA) solutio.[Nota-Si commercium obtinere non potest, agens Derivatio praeparari potest ut 1% singulae acido 3-mercaptopropionico et o-phthaldialdehyde in 0.4 M solutionem quiddam boratum.]
Solutio A: Translatio 4.1 g sodii acetatis trihydratis et 40 mg acidi ethylenediaminetetraacetici in 1-L uasi voluminis.Solve in aquae 950 mL, et compone cum 0.1 N hydroxide sodium ad pH 7.2.Aqua diluto volumine, tetrahydrofuran adde 2.5 mL, et misce.Colum, degas.
Solutio B: Translatio 2.7 g trihydratorum sodii acetatis et 40 mg EDTA in lagenam voluminis 1-L.200 mL aquae solve et cum 0.1 N hydroxide sodium ad pH 7.2.Adde 800 mL ex acetonitrile, sparguntur, et degas.
Mobile tempus: Vide infra mensam gradientem.
Solutio tempus (min) Solutio A (%) Solutio B (%)
0 96.7 3.3
20 60 40
24 0 100
38 0 100
38 96.7 3.3
45 96.7 3.3
Solutio mensurae: Transfer quantitatem ponderatam circiter 0.2 mg USP Orlistat Compositi E RS in phialam capitis 20-mL.Adde 10 mL 4 N hydroxidum sodium, et claude phialam.Ampullam ad 100 pro 1 h calefac, tunc refrigerandi ad cella temperiem permitte.Translatio 2 mL solutionis inde in lagena voluminis L-mL, et aqua ad volumen diluta.Ad huius solutionis 0.5 mL adde 2.0 mL Buffer et 0.5 mL agentis derivantis.
Sample solutio: Perge ad solutionem solutionis Standardi directam, sed pro 25 mg Orlistat utere ut restituas 0.2 mg USP Orlistat Compone E RS.
Systema chromatographicum
(Vide Chromatographiam <621>, Ratio idoneitatis.)
Modus: LC
Detector: Fluorescens 340 um (excitatio);450 um (emissio);
Columnae
Custodi: 2.1-mm × 2-cm;50-µm stipare L1
Analytica: 2.1-mm × 20-cm;stipare L1
Fluunt rate: 0.5 mL/min
Iniectio amplitudo: 20 µL
Ratio convenientia
Sample: Latin solution
Convenientia requisita
Relativum vexillum declinationis: NMT 6.0% pro orlistat affinis compositi E apicem
Analysis
Exempla: Standard solution et Sample solutionem
Recipis hanc immunditiam in portione Orlistat desumptam;
Proventus = (rU/rS) (CS/CU) 100
rU = apicem responsio pro compositis E orlistat relata in solutione Sample
rS = apicem responsio pro USP Orlistat Related Compone E RS in solutione Standard
CS = intentio USP Orlistat Composita E RS in Standard solutione (mg/mL)
CU = intentio Orlistat in solutione Sample (mg/mL)
Criteria acceptatio
Singula immunditia: NMT 0.2% orlistat affinis compositi E invenitur.
Totalis immunditiae: NMT 1.0% totalis immunditiae inventae sunt, proventus procedendi 1, 2, 3, 4, et 5 additis.
IN SPECIE TESTS
• Rotatio Optical, Rotatio Imprimis <781>
Sample solutio: 30 mg / mL in alcohole dehydratum
De acceptatione criteria: Inter -48.0 et -51.0, sub 20
• Determinatio aquae, Methodus Ic <921>: NMT 0.2%
ADDITICIUS REQUISITIS
• Packaging et Repono: Serva in vasis bene clausis inter 2 et 8℃.
• USP Signa Reference <11>
USP Orlistat RS
USP Orlistat Related Compone RS
USP Orlistat Related Compone B RS
USP Orlistat Related Compone C RS
USP Orlistat Related Compone D RS
USP Orlistat Related Compone E RS
USP35