Analysis

Specification

Result

Assay(C₁₇H₂₁NO₄ HBr)

99.0% Min

99.7%

Appearance

Colorless crystal or white Crystalline Powder

Complies

Specific rotation

-24-27

-25.3

Chemical reaction

(1), (2), (4) positive reaction

(3) infrared light absorption spectrum and the control patterns (spectrum, 288)

Are positive responses

Meet the requirements

Melting point

195~199℃

196℃

Solution clarification

Complies

Complies

PH

4.0-5.5

4.55

Other alkaloids

Complies

Complies

Easy oxide

Complies

Complies

Loss on Drying

13.0% Max

9.7%

Conclusion: Complies with the standard CP 2010.

Items

Specification

Result

Method

Appearance colour

White, almost white, colourless

Complies

Visual test

Appearance shape

Powder or crystals

Powder

Visual test

Solubility in ethanol 96%(V/V)

Freely soluble

Complies

Visual test

Solubility in water(Visual test)

Soluble

Complies

Visual test

Melting point

66-70℃

70℃

Capillary method

Specific optical rotation [alpha]20/D

calculated with reference to the solvent-free Substance

-39.0 - -33.0°

-36.2°

/

IR spectrum

Corresponding to

reference spectrum

Complies

IR spectrophotometry

UV spectrum

Corresponding to

reference spectrum

Complies

UV/VIS spectrophotometry

A 1%/1cm(257 nm)

calculated with reference to the solvent-free substance

5.9-6.5

6.1

UV/VIS spectrophotometry

Retention times

the retention time of the principal peak obtained with the test sample is the same as that obtained with the reference standard

Complies

HPLC

Liquid chromatography

Rf values principal spots

the Rf value of the principal spot obtained with the test substance must correspond to that

Complies

Thin-layer chromatography

Norscopolamine

0.5% Max

0.1%

Liquid chromatography

Any other Impurity

0.10% Max

0.05%

Liquid chromatography

Total of all Impurities

0.5% Max

0.1%

Liquid chromatography

Total of all subsidiary spots

0.5% Max

0.5%

TLC

Any other impurity

0.10% Max

0.05%

Liquid chromatography

tert. -butyl methyl ether

3000ppm Max

700ppm

GC

Total of 2-methyl-1-butanol and 3-methyl-1-butanol

500ppm Max

50ppm

GC

Toluene

100ppm Max

10ppm

GC

Pentanol-1

500ppm Max

50ppm

GC

Analytical procedure

not supplied

Meets the requirements

Complies

USP < 467 >

Water

0.5% Max

0.1%

Blamperometric Karl Fischer titration

Sulphated ash

0.1% Max

Complies

Limit test

Calculated with reference

to solvent-free substance

98.5-101.0%

99.3%

Titration

with perchloric acid

Calculated with reference

to solvent-free substance

99.0-100.5%

99.3%

Titration

with perchloric acid

Calculated with reference

to solvent-free substance

98.0-102.0%

99.3%

Liquid chromatography

Conclusion: Product corresponds with the requirements of current Ph.Eur.