ABSTRACT
Inserting chloramphenicol (CL) and hydrocortisone acetate (HCA) in cream preparation is intended to have activityagainst skin infection and dermatitis and such a product is available in the Indonesian market. Due to its capabilityas a separation technique, chromatography is widely used for the analysis of mixture in pharmaceutical products.The objective of this study was to develop high-performance liquid chromatography (HPLC) combined with anexperimental design for an effective analysis of CL and HCA in a cream formulation. In this study, the experimentalBox–Behnken design (BBD) was used. BBD is one of the useful experimental designs for the optimization ofchromatographic separation and analysis and for getting a better understanding of the interaction of studied factors onHPLC separation quality. Separation and HPLC analysis of CL and HCA were performed using a Shimadzu LC-20ADchromatograph, a Waters X-Bridge C-18 column (250 × 4.6 mm ID, 5 µm), and a UV-Vis detector at 261 nm. HPLCmethod was validated according to the International Conference on Harmonization by determining several analyticalperformances intended for the method’s purpose. Based on BBD, the optimal condition of HPLC was obtained usinga mobile phase of acetonitrile 47%– 53%, with a flow rate of 0.9 ml/minutes and a column temperature of 38°C. Thevalidation of HPLC resulted in the selectivity of a method with a resolution value of ≥1.5, linearity with a correlationcoefficient of >0.999, intraday and inter-day precisions with relative standard deviation values of ≤1.9%, and recoveryvalues in the range of 98%−102%. The validated method is successfully used for the analysis of CL and HCA in creamformulations. BBD could be an effective design to get the optimum reversed HPLC condition for the separation of CLand HCA in a cream formulation
ABSTRACT
Alpha-mangostin is the major component in Mangosteen (Garcinia mangostana Linn) pericarp having severalpharmacological activities including reducing blood pressure, antidiabetic, anticancer, and antioxidants. The objectiveof this study was to develop Fourier transform infrared spectroscopy-multivariate calibration of partial least square(PLS) for quantitative analysis of alpha-mangostin and to classify mangosteen pericarp using principal componentanalysis. Mangosteen pericarps from different locations (Java provinces and South Sulawesi, Republic of Indonesia)were extracted using ethanol and were subjected to high performance liquid chromatography (HPLC) for the analysisof alpha-mangostin and Fourier transform infrared (FTIR) spectroscopy measurements. HPLC was used to determinethe levels of alpha-mangostin and used as actual values during FTIR spectroscopy analysis. The prediction of alphamangostin was obtained from the correlation between actual values and FTIR predicted values and facilitated withthe PLS model. The results showed that the wavenumbers region of 3,825–937 cm−1 offered a reliable model with acoefficient correlation (r) value of 0.9927 and root mean square error of calibration of 0.0831%. The validation modelsalso exhibited the accurate and precise results for the prediction of alpha-mangostin with an r-value of 0.9754 androot mean square error of prediction value of 0.174%. Furthermore, the chemometrics of principal component analysisusing variables of absorbances at selected fingerprint (1,000–800 cm−1) could classify mangosteen pericarp fromdifferent regions. FTIR spectroscopy combined with chemometrics offered a reliable method for quality assurance ofmangosteen pericarp
ABSTRACT
The aim of this study was to optimize Fourier transform infrared (FTIR) spectroscopy and multivariate calibrationfor the quantitative analysis of Acid orange 7 (AO-7) and Sudan II (S-II) in blusher products. The calibration andvalidation samples were made by adding known concentrations of AO-7 and S-II in the placebo of blusher cosmeticsproducts. High-performance liquid chromatography equipped with photodiode array detector at 300–650 nm wasused to determine the actual values of AO-7 and S-II. The separation of AO-7 and S-II was performed using C18column at 40oC with mobile phase of acetonitrile-water in gradient elution program. FTIR spectra of evaluatedsamples were scanned using FTIR spectrophotometer equipped with attenuated total reflectance (ATR) samplingtechnique. The correlation between actual values of AO-7 and S-II as determined using high-performance liquidchromatography and FTIR predicted values was facilitated with multivariate calibrations. The selection of calibrationmodels relied on highest r2 and lowest levels of root mean square error of calibration, root mean square error ofprediction, and root mean square error of cross validation. The optimization results showed that FTIR spectra-partialleast square regression (PLSR) using wavenumbers of 3,450–2,400 cm−1 and six factors offered the highest r2 value(r2 > 0.98) and lowest errors. FTIR with ATR technique could be used to predict AO-7 and S-II in blusher product withthe main advantage of its simplicity, rapidity, and minimum sample preparation.
ABSTRACT
The objective of this study was to develop and to validate reversed-phase high-performance liquid chromatography(RP-HPLC) method for the determination of acid orange 7 (AO7) and Sudan II (SII) in blusher products. Separationof AO7 and SII was performed using C18 column (Thermo Synergy Gold 250 mm × 4.6 mm i.d., 5 µm) with mobilephase consisting of acetonitrile-water as a solvent (1:1 v/v) and delivered in gradient manner. The mobile phase wasdelivered at flow rate of 0.9 ml/minute, using column temperature of 40°C. RP-HPLC was validated by assessingseveral performance characteristics which included selectivity, linearity and range, sensitivity, precision, accuracy, androbustness. The developed RP-HPLC was selective for the separation of AO7 and SII. Over concentration of 10.326–41.304 µg/ml (AO7) and 9.967–39.869 (SII), the method was linear with coefficient of correlation (r) >0.999. Themethod was sensitive as indicated by low limit of detection and limit of quantification. The relative standard deviation(RSD) values during intra-assay and inter-assay were lower than those required by RSD Horwitz. The percentageof recovery was within acceptable ranges as required by Association of Official Analytical Chemists method. Thevalidated RP-HPLC method has been successfully applied for the analysis of AO7 and SII in commercial blusherproducts, and both AO7 and SII were not detected in the tested samples.
ABSTRACT
A novel of polymer combination promotes an increase of the ability for controlling the drug release. The objectiveof this research was to characterize the inter-polymer complexes (IPCs) of Eudragit (Eud) types (Eud RS, Eud L, orEud E) and Kollidon SR (KSR), and elucidate their effects on the drug release kinetics and mechanism. Differentpreparation techniques were proposed using spray drying and ultrasonic-assisted anti-solvent techniques. The thermalactivity, e.g., glass transition temperature (Tg) and Fourier transform infrared spectroscopy were used to characterizethe molecular interaction of these IPCs. Theophylline (THP) was selected as a drug model. The effect on the drugrelease kinetics and mechanism was the main concern of this study. Depending on the results, the hydrogen bondingformation between polymers was observed by a shifting of OH and carbonyl group vibrations. In addition, the van derWaals interaction was identified by an alteration in the vibrational band around the 1,000–1,500 cm−1. Meanwhile, thechange of physicochemical characteristic was identified by the Tg of IPCs. Eud E-KSR and Eud E-Eud L IPC wereunable to control the THP release. Meanwhile, Eud L-KSR IPC and Eud RS-KSR IPC were success to control theTHP release, but it was pH dependent and independent, respectively. This study concluded that the IPCs allowed theTHP release in a controlled manner based on the IPC characteristics and their interactions. Either positive or negativeinteractions on the drug release were observed due to native characteristics of polymers.
ABSTRACT
Herbal medicines along with its preparations have been commonly used as preventive and promotive agents around theworld, especially in developing countries. Motivated by economic profits, the high-priced value of herbal medicinesmay be substituted or adulterated with less expensive ones; therefore, the authentication methods must be developedto overcome the adulteration practices. Due to their properties as fingerprint analytical techniques, near-infrared (NIR)and mid-infrared (MIR) spectroscopies offered fast and reliable techniques for authentication of herbal medicine.The data generated during authentication of herbal medicines were complex and difficult to be interpreted; therefore,the statistical approach called chemometrics has been used to treat data. The objective of the present review was tohighlight the updates on the application of NIR and MIR spectroscopies and chemometrics techniques (discrimination,classification, and quantification) for discrimination and authentication of herbal medicine