跪求usp40标准

wsr1998

各位大神求助：求usp40地索奈德原料Desonide标准，跪谢！

宝宝小七

Desonide(des' oh nide).

[url=][/url]

C24H32O6 416.51
Pregna-1,4-diene-3,20-dione, 11,21-dihydroxy-16,17-[(1-methylethylidene)bis(oxy)]-, (11β,16α)-;     
11β,16α,17,21-Tetrahydroxypregna-1,4-diene-3,20-dione cyclic 16,17-acetal with acetone           [638-94-8].
UNII: J280872D1O   
DEFINITION
Desonide contains NLT 98.0% and NMT 102.0% of the labeled amount of desonide (C24H32O6 ), calculated on the dried basis.


IDENTIFICATION
•  A. Infrared Absorption 〈197K〉
•  B. The retention time of the major peak of the Sample solution corresponds to that of the Standard solution, as obtained in the Assay.
ASSAY
•  ProcedureUse low-actinic glassware for all solutions containing desonide.

Solution A: 0.1% Phosphoric acid in water
Solution B: Acetonitrile
Mobile phase: See Table 1.

Table 1

Time
(min)

Solution A
(%)

Solution B
(%)

0

70

30

4

68

32

5

68

32

9

65

35

13

30

70

16

30

70

Diluent: Solution A and acetonitrile (60:40)
System suitability solution: 0.7 mg/mL of USP Desonide Impurities Mixture RS in Diluent
Standard solution: 0.7 mg/mL of USP Desonide RS in Diluent
Sample solution: 0.7 mg/mL of Desonide in Diluent
Chromatographic system (See Chromatography 〈621〉 , System Suitability.)

Mode: LC
Detector: UV 254 nm
Column: 4.6-mm × 15-cm; 2.6-μm packing L7
Temperatures Column: 20° (15° –22° was shown to be acceptable)
Autosampler: 20°

Flow rate: 1 mL/min
Injection volume: 5 μL

System suitability Samples: System suitability solution and Standard solution
Suitability requirements Resolution: NLT 2.0 between desonide glyoxal and deoxyprednisolone-16-ene; NLT 2.0 between desonide and dihydrodesonide, System suitability solution
Relative standard deviation: NMT 0.73%, Standard solution


Analysis Samples: Standard solution and Sample solution
Calculate the percentage of desonide (C24H32O6 ) in the portion of Desonide taken:

Result = ( r U / r S ) × ( C S / C U ) × 100

r U	=	peak response from the Sample solution
r S	=	peak response from the Standard solution
C S	=	concentration of USP Desonide RS in the Standard solution (mg/mL)
C U	=	concentration of Desonide in the Sample solution (mg/mL)

Acceptance criteria: 98.0%–102.0% on the dried basis

IMPURITIES
•   Residue on Ignition 〈281〉 : NMT 0.10%
•  Organic ImpuritiesSolution A, Solution B, Mobile phase, Diluent, System suitability solution, Standard solution, Sample solution, and Chromatographic system: Proceed as directed in the Assay.
Sensitivity solution: 0.28 μg/mL of USP Desonide RS in Diluent from the Standard solution
System suitability Samples: System suitability solution and Sensitivity solution
Suitability requirements Resolution: NLT 2.0 between desonide glyoxal and deoxyprednisolone-16-ene; NLT 2.0 between desonide and dihydrodesonide, System suitability solution
Signal-to-noise ratio: NLT 10, Sensitivity solution


Analysis Sample: Sample solution
Calculate the percentage of each impurity in the portion of Desonide taken:

Result = ( r U / r T ) × (1/F) × 100

r U	=	peak area of each impurity from the Sample solution
r T	=	total peak area from the Sample solution
F	=	relative response factor (see Table 2)

Acceptance criteria: See Table 2.[Note— Disregard peaks that are less than 0.04% of the desonide peak from the Standard solution. ]

Table 2

Name

Relative
Retention
Time

Relative
Response
Factor

Acceptance
Criteria,
NMT (%)

16α-Hydroxyprednisolonea

0.31

1.0

0.15

Prednisoloneb

0.48

1.0

0.15

Desonide glyoxalc

0.76

1.0

0.50

Deoxyprednisolone-16-ened

0.82

1.7

0.50

Sum of desonide glyoxal and deoxyprednisolone-16-ene

—

—

0.50

Desonide

1.00

—

—

Dihydrodesonidee

1.07

0.84

0.50

Epoxydesonidef

1.18

1.0

0.50

Sum of dihydrodesonide and epoxydesonide

—

—

0.50

Bromodesonideg

1.43

0.68

0.15

Acetyldesonideh

1.74

0.82

0.15

Any other impurity

—

1.0

0.10

Total impurities

—

—

1.0

a  11β,16α,17,21-Tetrahydroxy-3,20-dioxopregna-1,4-diene.
b  11β,17,21-Trihydroxy-3,20-dioxopregna-1,4-diene.
c  11β-Hydroxy-16α,17-[(1-methylethylidene)bis(oxy)]-3,20-dioxopregna-1,4-dien-21-al.
d  11β,21-Dihydroxypregna-1,4,16-triene-3,20-dione.
e  11β,21-Dihydroxy-16α,17-[(1-methylethylidene)bis(oxy)]pregn-4-ene-3,20-dione.
f  9,11β-Epoxy-21-hydroxy-16α,17-(1-methylethylidenedioxy)pregna-1,4-diene-3,20-dione.
g  9α-Bromo-11β,21-dihydroxy-16α,17-[(1-methylethylidene)bis(oxy)]pregna-1,4-diene-3,20-dione.
h  11β-Hydroxy-16α,17-[(1-methylethylidene)bis(oxy)]-3,20-dioxopregna-1,4-dien-21-yl acetate.

SPECIFIC TESTS
•   Loss on Drying 〈731〉Sample: 1.0 g
Analysis: Dry at 105° for 3 h.
Acceptance criteria: NMT 0.5%

•   Optical Rotation, Specific Rotation 〈781S〉Sample: 10 mg/mL in dioxane
Acceptance criteria: +104.0° to +110.0°, calculated on the dried basis

ADDITIONAL REQUIREMENTS
•  Packaging and Storage: Preserve in tight containers, and store at controlled room temperature. Protect from light.
•   USP Reference Standards 〈11〉USP Desonide RS
USP Desonide Impurities Mixture RSThis is a mixture that contains desonide and may contain about 1% each of 16α-hydroxyprednisolone, prednisolone, desonide glyoxal, deoxyprednisolone-16-ene, dihydrodesonide, epoxydesonide, bromodesonide, and acetyldesonide.