Detection of indomethacin by high-performance liquid chromatography with in situ electrogenerated Mn(III) chemiluminescence detection.
The determination of indomethacin (INM) in pharmaceutical and biological samples by means of high-performance liquid chromatography (HPLC) with in situ electrogenerated Mn(III) chemiluminescence (CL) detection was proposed. The method was based on the direct CL reaction of INM and Mn(III), which was in situ electrogenerated by constant current electrolysis. The chromatographic separation was carried out on Nucleosil RP-C(18) column (250 mm x 4.6 mm; i.d., 5 microm; pore size, 100 A) at 20 degrees C. The mobile phase consisted of methanol:water:acetic acid=67:33:0.1 solution. At a flow rate of 1.0 mL min(-1), the total run time was 10 min. The effects of several parameters on the HPLC resolution and CL emission were studied systematically. Under the optimal conditions, a linear range from 0.01 to 10 microg mL(-1)(R(2)=0.9991), and a detection limit of 8 ng mL(-1) (signal-to-noise ratio=3) for INM were achieved. The relative standard deviations (R.S.D.) for 0.1 microg mL(-1) INM were 2.2% within a day (n=11) and 3.0% on 5 consecutive days (n=6), respectively. The recovery of INM from urine samples was more than 92%. The applicability of the method for the analysis of pharmaceutical and biological samples was examined.
Zhang
Yantu
Y
College of Chemistry and Materials Science, Shaanxi Normal University, Xi'an 710062, China.
Zhang
Zhujun
Z
Qi
Guangcai
G
Sun
Yonghua
Y
Wei
Yue
Y
Ma
Hongyan
H
D000894:Anti-Inflammatory Agents, Non-Steroidal / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid; D007213:Indomethacin / Q000032:analysis*; D049449:Luminescence; D008345:Manganese / Q000737:chemistry*; D015203:Reproducibility of Results
D000894:Anti-Inflammatory Agents, Non-Steroidal; D008345:Manganese; D007213:Indomethacin