ABSTRACT
The characteristics, performance, and application of an electrode, namely Pt|Hg|Hg(2)(DCF)(2)|graphite, where DCF stands for diclofenac ion, are described. This electrode responds to diclofenac with sensitivity of (58.1+/-0.8)mV/decade over the range 5.0 x 10(-5) to 1.0 x 10(-2)mol l(-1) at pH 6.5-9.0 and a detection limit of 3.2 x 10(-5)mol l(-1). The electrode is easily constructed at a relatively low cost with fast response time (within 10-30s) and can be used for a period of 5 months without any considerable divergence in potentials. The proposed sensor displayed good selectivity for diclofenac in the presence of several substances, especially concerning carboxylate and inorganic anions. It was used to determine diclofenac in pharmaceutical preparations by means of the standard additions method. The analytical results obtained by using this electrode are in good agreement with those given by the United States Pharmacopeia procedures.
ABSTRACT
A flow-injection spectrophotometric procedure is proposed for methyldopa determination in pharmaceutical preparations. The determination is based on formation of a yellow product (measured at 410nm) after complexation of methyldopa with molybdate. Under optimal conditions, Beer's law is obeyed in a concentration range of 50-200mgl(-1) methyldopa. Typical correlation between absorbance and analyte concentration was 0.9999. Usual excipients used as additives in pharmaceuticals do not interfere with the proposed method. The analytical frequency was 210h(-1) and the relative standard deviation (R.S.D.) was
ABSTRACT
The characteristics, performance, and application of an electrode, namely, Pt|Hg|Hg(2)(PABzt)(2)| graphite, where PABzt stands for p-aminobenzoate ion, are described. This electrode responds to PABzt with sensivity of (58.1+/-1.0) mV per decade over the range 1.0x10(-4) to 1.0x10(-1)moll(-1) at pH 6.5-8.0 and a detection limit of 3.2x10(-5)moll(-1). The electrode shows easy construction, fast response time (within 10-30s), low-cost, and excellent response stability (lifetime greater than 6 months, in continuous use). The proposed sensor displayed good selectivity for p-aminobenzoate in the presence of several substances, especially, concerning carboxylate and inorganic anions. It was used to determine p-aminobenzoate in pharmaceutical formulations by means of the standard additions method. The results obtained by using this electrode compared very favorably with those given by an HPLC procedure.
ABSTRACT
In this report an analytical method to determine furosemide by using diffuse reflectance spectroscopy is presented. This study shows that this technique can give quantitative results using spot test analysis, particularly in the case of pharmaceuticals containing furosemide. The color spot test could be obtained by reaction between furosemide with p-dimethylaminocinnamaldehyde, in acid medium. This reaction produced a stable complex on filter paper after heating to 80 degrees C for 5min. All reflectance measurements were carried out at 585nm and the linear range was from 7.56x10(-3) to 6.05x10(-2)moll(-1), with a correlation coefficient of 0.999. The limit of detection was estimated to be 2.49x10(-3)moll(-1) (R.S.D.=1.7%) and the effect of common excipients on the reflectance measurements was evaluated. The method was applied to determine furosemide in commercial brands of pharmaceuticals. The results obtained by the proposed method were favorably compared with those of the official method, showing for the first time ever that quantitative spot test analysis by diffuse reflectance could be successfully used to determine furosemide in tablets.
ABSTRACT
The procedure for formaldehyde analysis recommended by the National Institute for Occupational Safety and Health (NIOSH) is the Chromotropic acid spectrophotometric method, which is the one that uses concentrated sulphuric acid. In the present study the oxidation step associated with the aforementioned method for formaldehyde determination was investigated. Experimental evidence has been obtained indicating that when concentrated H(2)SO(4) (18 mol l(-1)) is used (as in the NIOSH procedure) that acid is the oxidizing agent. On the other hand, oxidation through dissolved oxygen takes place when concentrated H(2)SO(4) is replaced by concentrated hydrochloric (12 mol l(-1)) and phosphoric (14.7 mol l(-1)) acids as well as by diluted H(2)SO(4) (9.4 mol l(-1)). Based on investigations concerning the oxidation step, a modified procedure was devised, in which the use of the potentially hazardous and corrosive concentrated H(2)SO(4) was eliminated and advantageously replaced by a less harmful mixture of HCl and H(2)O(2).
