Promazine Hydrochloride
;)
10H-Phenothiazine-10-propanamine,N,N-dimethyl-,monohydrochloride.
10-3-(Dimethylamino)propylphenothiazine monohydrochloride [53-60-1].
»Promazine Hydrochloride,dried at 105
for 2hours,contains not less than 98.0percent and not more than 102.0percent of C17H20N2S·HCl.
for 2hours,contains not less than 98.0percent and not more than 102.0percent of C17H20N2S·HCl.
Packaging and storage—
Preserve in tight,light-resistant containers.
Completeness and clarity of solution—
Asolution of it (1in 10)and a 1in 10solution of it in chloroform are practically clear and show not more than a light yellow color.
NOTE—Throughout the following procedures,protect test or assay specimens,the Reference Standard,and solutions containing them,by conducting the procedures without delay,under subdued light,or using low-actinic glassware.
Identification—
A:
Infrared Absorption á197Kñ.
B:
Determine the absorbance of the assay solution employed for measurement of absorbance in the Assayat 301nm,using 0.1Nhydrochloric acid as the blank.Similarly determine the absorbance of a 1in 10dilution of this solution,prepared with the same acid,at the wavelength of maximum absorbance at about 252nm:the ratio 10(A252/A301)is between 7.1and 7.9.
C:
It responds to the tests for Chloride á191ñ.
Melting range,Class Iá741ñ:
between 172and 182,but the range between beginning and end of melting does not exceed 3.
and 182,but the range between beginning and end of melting does not exceed 3.
pHá791ñ:
between 4.2and 5.2,in a solution (1in 20).
Loss on drying á731ñ—
Dry it at 105for 2hours:it loses not more than 0.5%of its weight.
for 2hours:it loses not more than 0.5%of its weight.
Residue on ignition á281ñ:
not more than 0.1%.
Selenium á291ñ—
The absorbance of the solution from the Test Solution,prepared with 100mg of Promazine Hydrochloride and 200mg of magnesium oxide,is not greater than one-half that from the Standard Solution(0.003%).
Heavy metals,Method IIá231ñ:
0.005%.
Chromatographic purity—
[NOTE—Perform this test under conditions of subdued light and with no unnecessary delays between the preparation of the solutions and the development of the chromatographic plate.]
Developing solvent—
Mix 95volumes of toluene with 15volumes of alcohol and 1volume of ammonium hydroxide.
Standard preparations—
Dissolve an accurately weighed quantity of USP Promazine Hydrochloride RSin methanol to obtain Standard preparation Ahaving a known concentration of 0.4mg per mL.Dilute quantitatively with methanol to obtain Standard preparationshaving the following compositions:
| Standard preparation |
Dilution | Concentration (µg RSper mL) |
Percentage (%, for comparison with test specimens) |
| A | (undiluted) | 400 | 2.0 |
| B | (1in 2) | 200 | 1.0 |
| C | (3in 10) | 120 | 0.6 |
| D | (1in 10) | 40 | 0.2 |
Test preparation—
Dissolve an accurately weighed quantity of Promazine Hydrochloride in methanol to obtain a solution containing 20mg per mL.
Procedure—
Apply separately 10µLof the Test preparationand 10µLof each Standard preparationto a suitable thin-layer chromatographic plate (see Chromatography á621ñ)coated with a 0.25-mm layer of chromatographic silica gel mixture ,and allow to dry.Position the plate in a chromatographic chamber and develop the chromatograms in the Developing solventuntil the solvent front has moved about three-fourths of the length of the plate.Remove the plate from the developing chamber,mark the solvent front,and allow the solvent to evaporate by air drying for 15minutes.Examine the plate under short-wavelength UVlight.Compare the intensities of any secondary spots observed in the chromatogram of the Test preparationwith those of the principal spots in the chromatograms of the Standard preparations:the sum of the intensities of secondary spots obtained from the Test preparationcorresponds to not more than 2.0%of related compounds,with no single impurity corresponding to more than 1.0%.
Organic volatile impurities,Method Iá467ñ:
meets the requirements.
Assay—
[NOTE—Use low-actinic glassware.]Transfer about 50mg of Promazine Hydrochloride,previously dried and accurately weighed,to a 1000-mLvolumetric flask,add 0.1Nhydrochloric acid to volume,and mix.Without delay,concomitantly determine the absorbances of this solution and of a Standard solution of USP Promazine Hydrochloride RSin the same medium having a known concentration of about 50µg per mLin 1-cm cells at the wavelength of maximum absorbance at about 301nm,with a suitable spectrophotometer,using 0.1Nhydrochloric acid as the blank.Calculate the quantity,in mg,of C17H20N2S·HCl in the portion of Promazine Hydrochloride taken by the formula:
C(AU/AS),
which Cis the concentration,in µg per mL,of USP Promazine Hydrochloride RSin the Standard solution,and AUand ASare the absorbances of the solution of Promazine Hydrochloride and the Standard solution,respectively.
Auxiliary Information—
Staff Liaison:Karen A Russo,Ph.D.,Scientist
Expert Committee:(PA1)Pharmaceutical Analysis 1
USP28–NF23Page 1639
Pharmacopeial Forum:Volume No.29(5)Page 1566
Phone Number:1-301-816-8379