Facile LC‐UV methods for simultaneous monitoring of ciprofloxacin and rosuvastatin in API, formulations and human serum

Abstract

An efficient, selective and cost-effective liquid chromatographic assay was developed and validated for the simultaneous quantification of ciprofloxacin and rosuvastatin in Active Pharmaceutical Ingredients (API), pharmaceutical formulations and in human serum. The chromatographic system consisted of mobile phase methanol-water, 90:10 v/v at pH 3.0 adjusted with o-phosphoric acid, pumped at 1.0 mL/min through a prepacked Purospher Star C18 (5 µm, 25 × 0.46 cm) column and effluent was monitored at the isosbestic point (255 nm) as well as at the λmax of individual drugs (243 and 271 nm). The method was validated over a linear concentration range of 0.25-15 µg/mL for ciprofloxacin and 0.33-20 µg/mL for rosuvastatin (r(2) ≥ 0.999). The ranges of reliable response (limits of detection and quantitation) for ciprofloxacin were 3-15 and 9-45 ng/mL and 17-29 and 52-88 ng/mL, respectively, for rosuvastatin in all API, pharmaceutical formulations and human serum. Analytical recovery from human serum was >98% and relative standard deviation (RSD) was <2. The accuracies were 97.13-102.55 and 97.41-101.31% and precisions in RSD were 0.04-1.90 and 0.02-1.23% for ciprofloxacin and rosuvastatin, respectively. No matrix interferences, ion suppression/enhancement and carry-over were detected. The total assay run time was less than 5 min. In another study, for optimum performance the detector was programmed for multiwavelength scanning at the absorption maxima of each component. Consequently, the linearity range was improved and limit of detection and quantitation values were down to 1-4 and 4-12 ng/mL for ciprofloxacin and 3-5 and 9-15 ng/mL for rosuvastatin, respectively. The validation parameters fitted ICH guidelines through the isosbestic and individual λmax approach. The small sample volume and simplicity of preparation make this method suitable for use in human serum samples, pharmaceutical formulations, quality control, drug-drug interaction studies, clinical laboratories, drug research centers and forensic medical centers.

Quantitation of Ciprofloxacin by RP-HPLC from Active and Dosage Formulations

“…Many methods have already been reported for estimations of ciprofloxacin [6][7][8][9][10][11][12] and but the present method is straightforward and is validated according to ICH (International Conference on Harmonization) guidelines [16]. All of the parameters were found under the limits of ICH guidelines, and the chromatogram of the analyte revealed that the method was specific and no peak of internal standard interfered, and can be considered selective.…”

“…suppositories, gels, eye drops, etc.) [6][7][8][9][10][11][12]. A direct and sensitive HPLC method for determining ciprofloxacin in the influenza vaccine has been described [7] employing a mobile phase of acetonitrile/water/phosphoric acid.…”

“…The separation was achieved using a mobile phase of methanol-water at a ratio of 90:10 v/v. The flow rate was 1 mLmin -1 , the pH of the mobile phase was pH 3, and drugs were monitored at 255 nm [9]. Similarly, an HPLC-UV method was described for the determination of ciprofloxacin in human plasma with a phosphate buffer (pH 2.7) and acetonitrile (77:23, v/v), and the drug was detected at 277 nm [10,[13][14][15].…”

A simple, rapid and fully validated HPLC method for simultaneous quantitative bio‐analysis of rosuvastatin and candesartan in rat plasma: Application to pharmacokinetic interaction study

“…A literature review revealed several bio‐analytical methods reported for ROS (Braga, Mancila, Cassella, & Pacheco, ; Caglar & Toker, ; Darwish & Al‐malaq, ; J. Gao, Zhong, Duan, & Chen, ; C K Hull, Penman, Smith, & Martin, ; Caroline K. Hull, Martin, Warwick, & Thomas, ; Hussain, Patel, & Tan, ; Kallem, Karthik, Chakradhar, & Mullangi, ; T. R. Kumar et al, ; Lan et al, ; H. K. Lee, Ho, Hu, Tomlinson, & Wong, ; MacWan, Ionita, & Akhlaghi, ; Oudhoff, Sangster, Thomas, & Wilson, ; Xu, Ruan, Yuan, & Jiang, ) and CAN (Gao et al, ; Jeon et al, ; Kondo, Yoshida, Yoshimura, Motohashi, & Tanayama, ; J. W. Lee et al, ; Lou, Ruan, & Jiang, ; Miyabayashi, Okuda, Motohashi, Izawa, & Yashiki, ; Prajapati, Patel, Chauhan, Patel, & Patel, ; Stenhoff, Lagerström, & Andersen, ) individually or in combination with other drugs like pioglitazone, hydrochlorothiazide, ciprofloxacin, metformin, etc., using either HPLC or LC–MS/MS (Arayne, Sultana, & Tabassum, ; Pp. Kumar, Murthy, & Basaveswara Rao, ; Narapusetti, Bethanabhatla, Sockalingam, Repaka, & Saritha, ; Nasir et al, ; Shah et al, ; Trivedi, Kallem, Mullangi, & Srinivas, ; Varghese & Ravi, ; Vittal et al, ; Bharathi, Hotha, Chatki, Satyanarayana, & Venkateswarlu, ; Gonzalez, Lopez, Alonso, & Jimenez, ; Kumari Karra, Rao Pilli, Kumar Inamadugu, & Seshagiri Rao, ; Nie et al, ; Singh, Lokhandae, Dwivedi, Sharma, & Dubey, ).…”