Abstract
A reverse phase stability indicating HPLC method for simultaneous determination of two antispasmodic drugs in pharmaceutical parenteral dosage forms (injectable) and in serum has been developed and validated. Mobile phase ingredients consist of Acetonitrile : buffer : sulfuric acid 0.1 M (50 : 50 : 0.3 v/v/v), at flow rate 1.0 mL/min using a Hibar μBondapak ODS C18 column monitored at dual wavelength of 266 nm and 205 nm for phloroglucinol and trimethylphloroglucinol, respectively. The drugs were subjected to stress conditions of hydrolysis (oxidation, base, acid, and thermal degradation). Oxidation degraded the molecule drastically while there was not so much significant effect of other stress conditions. The calibration curve was linear with a correlation coefficient of 0.9999 and 0.9992 for PG and TMP, respectively. The drug recoveries fall in the range of 98.56% and 101.24% with 10 pg/mL and 33 pg/mL limit of detection and limit of quantification for both phloroglucinol and trimethylphloroglucinol. The method was validated in accordance with ICH guidelines and was applied successfully to quantify the amount of trimethylphloroglucinol and phloroglucinol in bulk, injectable form and physiological fluid. Forced degradation studies proved the stability indicating abilities of the method.
Highlights
Phloroglucinol (1,3,5-trihydroxybenzene, PG) and its methylated derivative tri-O-methylphloroglucinol (TMP), Figure 1, are established pharmaceutical agents inhibit the action of catechol-O-methyl transferase, inducing relaxation of smooth muscles, and decreasing glycerolinduced abdominal pain and are characterized by a swift and strong spasmolytic activity, relieving pain
Limit of detection and quantification (LOD and Limit of quantification (LOQ)) for the method were established by sequentially diluting the standard solutions at decreasing concentrations, in the range of 100–1 pg/mL for PG and 10–1 pg/mL for TMP
The high-performance liquid chromatography (HPLC) method development and its validation are the prioritized requirements for any drug available in the market to ensure the quality of the products
Summary
Phloroglucinol (1,3,5-trihydroxybenzene, PG) and its methylated derivative tri-O-methylphloroglucinol (TMP), Figure 1, are established pharmaceutical agents inhibit the action of catechol-O-methyl transferase, inducing relaxation of smooth muscles, and decreasing glycerolinduced abdominal pain and are characterized by a swift and strong spasmolytic activity, relieving pain. Literature survey reveals that some of the analytical methods for phloroglucinol are available including extraction and high-performance liquid chromatography (HPLC) [8,9,10], HPLC-mass spectrometry [11, 12], gas chromatographymass spectrometry [13], and spectrophotometry [14]. There is no simple and sensitive method to be followed on industrial basis especially in general quality control laboratories. They cannot be followed in the laboratories those of third world countries. The purpose of this write-up is to suggest a systematic approach for the development of a validated simple, sensitive, and stability indicating RP-HPLC method that should meet the current ICH and regulatory requirements [22]
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