Validated HPLC and stability-indicating densitometric chromatographic methods for simultaneous determination of camylofi
- PDF / 1,931,470 Bytes
- 11 Pages / 595.276 x 790.866 pts Page_size
- 1 Downloads / 205 Views
ORIGINAL PAPER
Validated HPLC and stability‑indicating densitometric chromatographic methods for simultaneous determination of camylofin dihydrochloride and paracetamol in their binary mixture Sawsan A. Abdel Razeq1 · Israa A. Khalil1 · Samah A. Mohammd2 Received: 7 January 2020 / Accepted: 16 May 2020 © Iranian Chemical Society 2020
Abstract Two accurate, sensitive, precise and selective HPLC and stability-indicating TLC methods were developed for the simultaneous determination of camylofin-2HCl and paracetamol. Forced acid, alkali and oxidative degradation of camylofin2HCl were tried where complete degradation was achieved using 5 N HCl. HPLC method was developed to determine the mixture of the two drugs using Zorbax N H2 column and a mobile phase of 0.5% triethylamine and pH 3.0 adjusted with 0.1% phosphoric acid and methanol (70:30 v/v) over concentration ranges of 3–90 and 10–95 µg/mL for camylofin-2HCl and paracetamol, respectively.TLC method was used for the separation of camylofin from its acid degradate and paracetamol using chloroform–methanol–acetone–conc. ammonia (8:2:2:0.1, by volume) as developing system and band scanning at 254 nm over concentration ranges of 5–40 µg/band for camylofin-2HCl and 0.1–0.5 µg/band for paracetamol. The validation of two methods was carried out according to ICH guideline. Accuracy ranged between 98.47 and 100.67% for the two methods with acceptable precision RSD% ranging between 0.66 and 1.47%. Keywords Camylofin · Paracetamol · Acidic degradate · HPLC · TLC densitometry
Introduction Camylofin-2 HCl (3-methyl butyl 2-(2-diethyl amino ethyl amino)-2-phenyl acetate hydrochloride) is a part of anticholinergic, spasmolytic and gastrointestinal sedative group [1, 2]. It is found in market as single or combined formulation with paracetamol, nimesulide, diclofenac and analgin. The literature revealed many analytical techniques for the quantification of camylofin-2HCl such as spectrophotometry [3, 4], HPLC [5–9] TLC densitometry [6, 7, 10–12] and GC [13, 14]. Paracetamol (N-acetyl-para-amino-phenol) has antipyretic and analgesic action and weak anti-inflammatory effect [1]. Many techniques have been used for its determination, including spectrophotometry [15–17], HPLC [18–21] TLC * Israa A. Khalil [email protected] 1
Analytical Chemistry Department, Faculty of Pharmacy (Girls), Al-Azhar University, Cairo, Egypt
National Organization for Drug Control and Research (NODCAR), Giza, Egypt
2
[22–25], GC [26–29], fluorometry [30–32] and electrochemistry [33–36]. Literature review of the mixture analysis revealed that there are only two reported HPLC methods [37, 38] and one spectrophotometric method [39] which were developed for the determination of both drugs simultaneously. But all the reported methods lack a sensitivity, and no reported TLC densitometric method for the simultaneous determination of camylofin-2HCl and paracetamol was developed up till now. The novelty of this work is the first development of TLC densitometric method for the determination of paracetamol
Data Loading...
