Thermal infrared enthalpimetry (TIE) was used for hypochlorite determination in commercial hypochlorite-based bleaching solutions. Experimental parameters were evaluated for the reaction with a hydrogen peroxide solution. The most relevant conditions were 5% H2O2 (m/m) solution, stirring speed of 250 rpm, dispensing rate of 0.57 mL s-1, and 10 s after reaction for the simultaneous temperature readings of four replicates. Agreement to reference method NBR 9425 ranging from 98.2 to 103.2% was achieved, with a low variation among measurements (relative standard deviation < 3.5%). The number of analytical operations was reduced, and only H2O2 solution was required as a greener reagent. A low amount of residues was generated (2.4 and 152.8 mL for each replicate in TIE and official method, respectively), and the application of the green analytical procedure index (GAPI) showed the greenness of the proposed method.

Abstract In this work, a simple and fast method is proposed for the determination of ethanol in homeopathic medicines using thermal infrared enthalpimetry (TIE). Samples containing alcohol in a wide concentration range (from 5% to 95% v/v) were used. Purified water or absolute ethanol was added directly into homeopathic medicine and increase of temperature was monitored using an infrared camera. Total volume, stirring speed and dispensing rate of solutions were the most significant parameters studied for method optimization. A response surface methodology (RSM) was used for optimization of the experimental conditions. The method was validated in the following parameters: selectivity, linearity, linear range, precision (repeatability and intermediate precision), limit of detection and quantification, accuracy and robustness. Linear range was obtained from 4% to 55% (ethanol, v/v). The proposed method showed accuracy in agreement with the conventional one. The proposed method it was demonstrated a good alternative for determination of ethanol in homeopathic medicines, presenting low cost, fast analysis and agreement with the principles of green analytical chemistry.

Content uniformity (CU) is a parameter used to ensure the uniformity of the amount of active substances in pharmaceutical preparations. It is often evaluated in the quality control of pharmaceutical dosage forms, and a novel method was proposed for CU determination using thermal infrared enthalpimetry (TIE). Captopril tablets were dissolved in 24-well microplates and the heat released from the reaction of captopril and I2 was monitored with an infrared camera. Some experimental parameters were adjusted, as captopril/I2 ratio, stirring speed and dispensing rate, and the most suitable conditions were 1.00:1.00 (v/v), 250 rpm and 0.57 mL s-1, respectively. Interferences from tablet adjuvants (e.g., starch, cellulose and lactose) were not observed. The results obtained by TIE did not differ statistically (Student’s t-test, p > 0.05) from those from official method (UV spectrophotometry) described in pharmacopeia. The TIE method required 31 and 12 times less reagent and time, respectively. Therefore, the proposed method was suitable for routine analysis and agrees with the requirements of green analytical chemistry.