Trimipramine Maleate
5H-Dibenz[b,f]azepine-5-propanamine, 10,11-dihydro-N,N, ![]() 5-[3-(Dimethylamino)-2-methylpropyl]-10,11-dihydro-5H-dibenz[b,f]azepine maleate (1:1) ![]() ![]() ![]() » Trimipramine Maleate contains not less than 98.0 percent and not more than 102.0 percent of C20H26N2·C4H4O4, calculated on the dried basis.
Packaging and storage
Preserve in tight containers, and store at room temperature.
USP Reference standards
![]() ![]() USP Iminodibenzyl RS ![]() USP Imipramine Hydrochloride RS. USP Trimipramine Maleate RS ![]() USP Trimipramine Related Compound A RS ![]()
Identification
B:
The retention time of the major peak in the chromatogram of the Assay preparation corresponds to that in the chromatogram of the Standard preparation, as obtained in the Assay.
Loss on drying
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Residue on ignition
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Heavy metals, Method II
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Related compounds
Mobile phase and Standard stock preparation
Prepare as directed in the Assay.
Impurity stock solution
Dissolve accurately weighed quantities of USP Imipramine Hydrochloride RS and USP Iminodibenzyl RS in a suitable volume of Mobile phase to obtain a solution having a known concentration of about 50 µg per mL of iminodibenzyl and 56.5 µg per mL of imipramine hydrochloride.
Trimipramine related compound A solution
Dissolve a suitable quantity of USP Trimipramine Related Compound A RS in Mobile phase to obtain a solution having a concentration of about 50 µg per mL.
Trimipramine stock solution
Quantitatively dilute the Standard stock preparation with Mobile phase to obtain a solution having a known concentration of about 70 µg per mL of trimipramine maleate.
System suitability solution
Transfer about 7 mg of USP Trimipramine Maleate RS to a 10-mL volumetric flask, dissolve in a small amount of Mobile phase, add 0.1 mL each of the Impurity stock solution and the Trimipramine related compound A solution, and dilute with Mobile phase to volume.
Standard solution
Transfer 5.0 mL each of the Impurity stock solution and the Trimipramine stock solution with Mobile phase to a 50-mL volumetric flask, and dilute with Mobile phase to volume. Dilute the resulting solution quantitatively, and stepwise if necessary, with Mobile phase to obtain a final solution having a known concentration of about 0.5 µg per mL each of iminodibenzyl, imipramine (free base), and trimipramine (free base). [noteThis solution is stable for one day at room temperature. The concentration of imipramine (free base), in µg per mL, can be calculated using the molecular weights of imipramine (282.41) and imipramine hydrochloride (318.88). The concentration of trimipramine (free base), in µg per mL, can be calculated using the molecular weights of trimipramine (294.43) and trimipramine maleate (410.51).]
Test solution
Use the Assay stock preparation.
Chromatographic system
Prepare as directed in the Assay. Chromatograph about 10 µL of the System suitability solution, and record the peak responses as directed for Procedure: the resolution, R, between imipramine and trimipramine related compound A is not less than 1.5. [noteFor identification purposes, the approximate relative retention times of the specified impurities are given in Table 1.]
Procedure
Separately inject about 10 µL of the Standard solution and the Test solution into the chromatograph, and record the chromatogram for three times the retention time for trimipramine. Identify the components based on their relative retention times in Table 1. Measure the peak areas of all the peaks in the Test solution. Calculate the percentage of imipramine and iminodibenzyl in the portion of Trimipramine Maleate taken by the formula:
100(CS / CT)(rU / rS)
in which CS is the concentration, in mg per mL, of any given impurity (free base) in the Standard solution; CT is the concentration of Trimipramine Maleate, in mg per mL, in the Test solution; rU is the individual peak response of the given impurity obtained from the Test solution; and rS is the corresponding response for the same impurity obtained from the Standard solution. Calculate the percentage of trimipramine related compound A in the portion of Trimipramine Maleate taken by the formula:
100(1/3.6)(CS / CT)(rU / rS)
in which 3.6 is the relative response factor for trimipramine related compound A; CS is the concentration, in mg per mL, of trimipramine (free base) in the Standard solution; CT is the concentration of Trimipramine Maleate, in mg per mL, in the Test solution; rU is the peak response for trimipramine related compound A obtained from the Test solution; and rS is the peak response of trimipramine obtained from the Standard solution. Calculate the percentage of each unknown impurity in the portion of Trimipramine Maleate taken by the formula:
100(CS / CT)(ri / rS)
in which CS is the concentration, in mg per mL, of trimipramine (free base) in the Standard solution; CT is the concentration of Trimipramine Maleate, in mg per mL, in the Test solution; ri is the individual peak response of the given impurity obtained from the Test solution; and rS is the response for trimipramine obtained from the Standard solution: the limits of the related compounds are given in Table 1. [noteDisregard any peak due to the maleate counterion eluting at a relative retention time of about 0.13.]
Table 1
Assay
Buffer solution
Dissolve about 1.4 g of anhydrous dibasic sodium phosphate in 1 L of water. Adjust with phosphoric acid to a pH of 7.7.
Mobile phase
Prepare a filtered and degassed mixture of acetonitrile, methanol, and Buffer solution (18:12:10). Make adjustments if necessary (see System Suitability under Chromatography
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Standard stock preparation
Dissolve an accurately weighed quantity of USP Trimipramine Maleate RS in a suitable volume of Mobile phase to obtain a solution having a known concentration of about 0.7 mg per mL.
Standard preparation
Transfer 3 mL of the Standard stock preparation to a 10-mL volumetric flask, and dilute with Mobile phase to volume to obtain a final solution having a known concentration of about 0.21 mg per mL of trimipramine maleate.
Assay stock preparation
Dissolve an accurately weighed quantity of Trimipramine Maleate in a suitable volume of Mobile phase to obtain a solution having a known concentration of about 0.7 mg per mL.
Assay preparation
Transfer 3 mL of the Assay stock preparation to a 10-mL volumetric flask, and dilute with Mobile phase to volume to obtain a final solution having a known concentration of about 0.21 mg per mL of trimipramine maleate.
Chromatographic system (see Chromatography
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Procedure
Separately inject equal volumes (about 20 µL) of the Standard preparation and the Assay preparation into the chromatograph, record the chromatograms for up to 1.5 times the retention time of trimipramine maleate, and measure the responses for the trimipramine maleate peak. Calculate the percentage of C20H26N2·C4H4O4, in the portion of Trimipramine Maleate taken by the formula:
100(CS / CU)(rU / rS)
in which CS is the concentration, in mg per mL, of USP Trimipramine Maleate RS in the Standard preparation; CU is the concentration, in mg per mL, of Trimipramine Maleate in the Assay preparation; and rU and rS are the trimipramine peak responses obtained from the Assay preparation and the Standard preparation, respectively.
Auxiliary Information
Please check for your question in the FAQs before contacting USP.
Chromatographic Column
USP32NF27 Page 3812
Pharmacopeial Forum: Volume No. 32(6) Page 1759
Chromatographic columns text is not derived from, and not part of, USP 32 or NF 27.
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