A Simple and Environmentally Friendly Reflectometric Method for the Rapid Quantitative Analysis of Captopril in Pharmaceutical Formulations
More details
Hide details
Centro de Ciências Sociais, Saúde e Tecnologia – UFMA, CEP 65900-000, Imperatriz, MA, Brazil
Instituto de Química – UNESP, P.O. Box 355, CEP 14801-970, Araraquara, SP, Brazil
Paulo Roberto S. Ribeiro   

Centro de Ciências Sociais, Saúde e Tecnologia – UFMA, CEP 65900-000, Imperatriz, MA, Brazil
Publish date: 2017-10-15
Eurasian J Anal Chem 2011;6(2):91–103
This paper describes a simple, environmentally friendly and rapid quantitative spot test procedure for the determination of captopril (CPT) in bulk drug and in pharmaceutical formulations by using diffuse reflectance spectroscopy. The proposed method is based on the reflectance measurements of the orange compound ( λmax 490 nm) produced by the spot test reaction between CPT and p-chloranil (CL). Under optimal conditions, calibration curves were obtained for CPT by plotting the optical density of the reflectance signal (AR) vs. the log of the mol L-1 concentration, from 6.91x10-3 to 1.17x10-1, with a good coefficient of determination (R2 = 0.9992). The common excipients used as additives in pharmaceuticals do not interfere in the proposed method. The method was applied to determine CPT in commercial pharmaceutical formulations. The results obtained by the proposed method are compared favorably with those obtained by an official procedure at 95% confidence level. The method validation results showed that the sensitivity and selectivity of the methods were adequated for drug monitoring in industrial quality control laboratories.
Florey K (1982) Analytical Profiles of Drug Substances, vol. 11, Academic Press: New York. p 81.
Gilman A G, Hardman J G, Limbird L E, Molinoff P B and Ruddon R W (2007) The Pharmacological Basis of Therapeutics, 11th Edition, MacGraw-Hill: New York. p 715.
Guerrero R S, Vives S S and Calatayud J M (1991) Fluorometric Determination of Captopril by Flow-Injection Analysis. Microchem J 43: 176.
Zhang X R, Baeyens W R G, Van Der Weken G, Calokerinos A C and Nakashima K (1995) Chemiluminescence Determination of Captopril Based on a Rhodamine-B Sensitized Cerium (IV) Method. Anal Chim Acta 303: 121.
Zhang Z D, Baeyens W R G, Zhang X R and Van Der Weken T (1996) Chemiluminescence flow-injection analysis of captopril applying a sensitized Rhodamine 6G method. J Pharm Biomed Anal 14: 939.
Xinrong Z, Baeyens W R G, Van Der Weken G, Calokerinos A C and Nakashima K (1995) Chemiluminescence analysis of captopril: comparison between luminol and rhodamine B-sensitized cerium(IV) methods. J Pharm Biomed Anal 13: 425.
Economou A, Themelis D G, Theodoridis G and Tzanavaras P D (2002) Sensitive determination of captopril by flow injection analysis with chemiluminescence detection based on the enhancement of the luminol reaction. Anal Chim Acta 463: 249.
El Walily A F M, Razak O A, Belal S F and Bakry R S (1999) Utilization of carbon disulfide for the analytical determination of betahistine hydrochloride and captopril in their pharmaceutical preparations. J Pharm Biom Anal 21: 439.
El Reis M A, Abou Attia F M and Kenawy I M M (2000) Indirect determination of captopril by AAS. J Pharm Biom Anal 23: 249.
Mirza T and Tan H S I (2001) Determination of captopril in pharmaceutical tablets by anion-exchange HPLC using indirect photometric detection; a study in systematic method development. J Pharm Biomed Anal 25: 39.
Kok R J, Visser J, Moolenaar F, Zeeuw D and Meijer D K F (1997) Bioanalysis of captopril: two sensitive high-performance liquid chromatographic methods with pre- or postcolumn fluorescent labeling. J Chromatogr B 693: 181.
Jankowski A, Skorek A, Krzyr ko K, Zarzycki P K, Ochocka R J and Lamparczyk H (1995) Captopril: determination in blood and pharmacokinetics after single oral dose. J Pharm Biomed Anal 13: 655.
Sypniewski S and Bald E (1996) Determination of captopril and its disulfides in whole human blood and urine by high-performance liquid chromatography with ultraviolet detection and precolumn derivatization. J Chromatogr A 729: 335.
Bald E and Sypniewski S (1997) Determination of thiol drugs in pharmaceutical formulations as their S-pyridinium derivatives by high-performance liquid chromatography with ultraviolet detection. Fresenius J Anal Chem 358: 554.
Cavrini V, Gatti R, Dipreta A M and Raggi M A (1987) HPLC determination of thio drugs in pharmaceutical formulations using ethacrynic acid as a precolumn ultraviolet derivatization reagent. Chromatographia 23: 680.
Cavrini V, Gotti R, Andrisano V and Gatti R (1996) 1,1'-[ethenylidenebis (sulfonyl)] bis-benzene: A useful pre-chromatographic derivatization reagent for HPLC analyses of thiol drugs. Chromatographia 42: 515.
Favaro G and Fiorani M (1996) Determination of pharmaceutical thiols by liquid chromatography with electrochemical detection: Use of an electrode with a conductive carbon cement matrix, chemically modified with cobalt phthalocyanine.
Liu YC, Wu H L, Kou H S, Chen S H and Wu S M (1995) Derivatization-gas chromatographic determination of captopril. Anal Lett 28: 1465.
Fraga J H G, Abizanda A I J, Moreno F J and Leon J J A (1998) Application of principal component regression to the determination of captopril by differential pulse polarography with no prior removal of dissolved oxygen. Talanta 46: 75.
Stefan R I, Van Staden J K F and Aboul-Enein H Y (2000) On-line assay of Scaptopril using an amperometric biosensor/sequential injection system. Anal Chim Acta 411: 51.
Palomeque M E and Band B S F (2002) Flow injection biamperometric determination of captopril. J Pharm Biomed Anal 30: 547.
Mohamed M E and Aboul – Enein H Y (1985) Amperometric and conductimetric method for simultaneous determination of captopril and bendroflumethiazide. Anal Lett 18: 2591.
United States Pharmacopeial Convention (2000) The United States Pharmacopeia: The national formulary; 24th ed.; Revision; Rockville. p. 296.
Mohamed M E, Aboul-Enein H Y and Gad-Kariem E A (1983) Potentiometric and visual titrimetric methods for analysis of captopril and its pharmaceutical forms. Anal. Lett. 16: 45.
El-Brashy A M (1995) Titrimetric determination of captopril in dosage forms. Acta Pharm Hung 65: 91.
Stefan R I, Van Staden J F and Aboul–Enein H Y (1999) A new construction for a potentiometric, enantioselective membrane electrode-its utilization to the Scaptopril assay. Talanta 48: 1139.
Pimenta A M, Araújo A N and Montenegro, M C B S M (2001) Sequential injection analysis of captopril based on colorimetric and potentiometric detection. Anal Chim Acta 438: 31.
Ribeiro P R S, Santini A O, Pezza H R and Pezza L (2003) Potentiometric determination of captopril in pharmaceutical formulations. Revista Eclética Química 28: 39.
Hillaert S and Van Den Bossche W (1999) Determination of captopril and its degradation products by capillary electrophoresis. J Pharm Biomed Anal 21: 65.
Nikolic K and Valasevic K S (1989) Conductometric determination of captopril. Pharmazie 44: 155.
Nikolic K and Valasevic K S (1991) Coulometric determination of captopril. Acta Pol Pharm 48: 5.
Sarna K and Fijalek Z (1997) Polarographic and voltammetric determination of captopril and captopril disulfide using a control grow mercury drop electrode. Chem Anal (Warsaw) 42: 425.
Askal H F (1991) New spectrophotometric methods for determination of captopril bulk drug and tablets. Talanta 10: 1155.
Ashour F M, Salama F M and Aziza M A E (1990) A colorimetric method for the determination of captopril. J Drugs Res 19: 323.
Albero M I, Sánchez-Petreño C, Garciá M S and Ródenas V (1993) Determination of captopril in pharmaceutical samples by flow-injection analysis. J Pharma Biom Anal 11: 887.
Jovanivic T, Stanovic B and Koricanac Z (1995) Spectrophotometric Investigation on Complex-Formation of Captopril with Palladium (II) and its Analytical Application. J Pharm Biomed Anal 13: 213.
Tzanavaras P D, Themelis D G, Economou A and Theodoridis G (2002) Reversed flow-injection manifold for the spectrophotometric determination of captopril based on its inhibitory effect on the Co(II)-2,2'-dipyridyl-2-pyridylhydrazone complex formation. Talanta 57: 575.
Sanghavi N M, Samarth M M, Matharu R and Singh P S (1991) Colorimetric estimation of captopril and its formulations. Indian Drugs 28: 189.
Sastry C S P, Sailaja A and Rao T T (1992) Determination of captopril by two simple spectrophotometric methods using oxidative coupling reaction. Pharmazie 46: 465.
Karlicek R and Solich P (1998) Flow-injection spectrophotometric determination of captopril using online solid phase extraction. Pharmazie 53: 549.
Dias N C, Porter M D and Fritz J S (2006) Principles and applications of colorimetric solid-phase extraction with negligible depletion. Anal Chim Acta 558: 230.
Feigl F and Anger V (1972) Spot Tests in Inorganic Analysis, 6th Edition, Elsevier Publishing Co.: Amsterdam. p 248.
los Weinert P, Pezza L and Pezza H R (2007) A Simplified Reflectometric Method for the Rapid Determination of Dipyrone in Pharmaceutical Formulations. J Braz Chem Soc 18: 846.
Rufino J L, Santos J M, Rodrigues M A, Pezza H R and Pezza L (2009) Determination of Ambroxol in Syrups Using Diffuse Reflectance Spectroscopy. Quim Nova 32: 1513.
Tubino M, Vitorino A R and De Magalhães M E A (1997) Quantitative spot tests of Fe(III), Cr(VI) and Ni(II) by reflectance measurements. Anal Lett 30: 271.
Gotardo M A, Gigante A C, Pezza L and Pezza H R (2004) Determination of furosemide in pharmaceutical formulations by diffuse reflectance spectroscopy Talanta 64: 361.
Ribeiro P R S, Pezza L and Pezza H R (2009) Determination of Methyldopa in Pharmaceutical Formulations by Combined Spot Test-Diffuse Reflectance Spectroscopy. J Braz Chem Soc 17: 674.
Pollo F, Sequinel R, Rufino J L, los Weinert P, Pezza H R and Pezza L (2009) An Environmentally Friendly Reflectometric Method for Bumetanide Determination in Pharmaceuticals. Anal Sci 25: 897.
Gotardo M A, Pezza L and Pezza H R (2005) Determination of Hydrochlorothiazide in Pharmaceutical Formulations by Diffuse Reflectance Spectroscopy. Revista Eclética Química 30: 17.
Reinecke D, Jensen A, Fister F and Scherman U (1988) Quantitative determination of organic compounds by diffuse reflectance Fourier Transform Infrared spectrometry. Anal. Chem. 60: 1221.
Narayanaswamy R and Sevilla F (1986) Reflectometric Study of the Acid-Base Equilibria of Indicators Immobilized on a Styrene Divinylbenzene Copolymer. Anal Chim Acta 189: 365.
Nakano N, Yamamoto A, Kobayashi Y and Nagashima K (1993) Development of a monitoring tape for hydrogen chloride gas using metanil yellow. Analyst 118: 1539.
Ghauch A, Turnar C, Fachinger C, Rima J, Charef A, Suptil J and Martin-Bouyer M (2000) Use of diffuse reflectance spectrometry in spot test reactions for quantitaive determination of cations in water. Chemosphere 40: 1327.
Dmitrienko S G, Sviridova O A, Pyatkova L N, Zhukova V A and Zolotov Y A (2000) Rapid determination of free active chlorine in water by diffuse reflectance spectroscopy after reaction with polyurethane foams. Anal Chim Acta 405: 231.
Ghauch A, Rima J, Charef A, Suptil J, Fachinger C and Martin-Bouyer M (1999) Quantitative measurements of ammonium, hydrogenophosphate and Cu (II) by diffuse reflectance spectrometry. Talanta 48: 385.
Kompany-Zareh M, Mansourian M and Ravaee F (2002) Simple method for colorimetric spot-test quantitative analysis of Fe(III) using a computer controlled hand-scanner. Anal Chim Acta 471: 97.
Savvin S B, Trutneva L M and Shvoeva O P (1993) Determination of chromium(VI) with diphenylcarbazide by diffuse reflection spectroscopy after preconcentration on disks of polyacrylonitrile fiber filled with a strongly basic anion-exchanger. J Anal Chim 48: 358.
Gazda D B, Fritz J S and Porter M D (2004) Multiplexed colorimetric solid-phase extraction: Determination of silver (I), nickel (II), and sample pH. Anal Chem 76: 4881.
Gazda D B, Lipert R J, Fritz J S and Porter M D (2004) Determination of nickel(II) as the nickel dimethylglyoxime complex using colorimetric solid phase extraction. Anal Chim Acta 510: 241.
Bebawy L I, El-Kousy N J, Suddik K and Shokry M (1999) Spectrophotometric determination of fluoxetine and sertraline using choloranil, 2,3-dichloro-5,6-dicyanobenzoquinone and iodine. J Pharm Biom Anal 21: 133.
Taha A and Rucker G (1977) Utility of pi-Acceptors in Alkaloid Assay. Arch Pharm 310: 485.
Long G L and Winefordner J D (1983) Limit of detection: a closer look at the IUPAC definition. Anal Chem 55: 712.
Foster R (1969) Organic Charge Transfer Complexes, Academic Press: London. P 335.
Miller J C and Miller J N (1993) Estadística para Química Analítica, 2nd Edition, Addison-Wesley Iberoamericana: Delaware. p 211.