Suma Ramagiri, Sarin R K, Saiprakash P K, Ramakrishna Sistla
Pharmacology Division, Indian Institute of Chemical Technology, Hyderabad, 500 007, India.
J Anal Toxicol. 2005 Oct;29(7):728-33. doi: 10.1093/jat/29.7.728.
This research paper describes the development and validation of an analytical method for the simultaneous determination of propoxur and isopropoxy phenol (IPP, a major metabolite) in both blood and urine of rat using reversed-phase high-performance liquid chromatography (HPLC) employing solid-phase extraction (SPE). Sample purification was performed using a weak cation-exchange cartridge (Isolute CBA). Separation was achieved by HPLC with UV detection at 270 nm. Recoveries of propoxur and IPP from blood and urine by SPE exceeded 85%. The validated calibration range for propoxur is from 0.5 to 100 microg/L and 2 to 100 microg/L for IPP in both rat blood and urine. The limit of quantitation for propoxur in blood and urine is 0.5 and 0.8 pg/L, respectively, and 2.0 and 4.2 microg/L, respectively, for IPP. Validation results on specificity, sensitivity, linearity, precision, accuracy, and stability are shown. The applicability of the method was demonstrated by the analysis of urine and blood from rats that were orally fed propoxur at minimum dose.
本研究论文描述了一种采用反相高效液相色谱法（HPLC）结合固相萃取（SPE）同时测定大鼠血液和尿液中残杀威及异丙氧基苯酚（IPP，一种主要代谢物）的分析方法的开发与验证。使用弱阳离子交换柱（Isolute CBA）进行样品净化。通过HPLC在270 nm处进行紫外检测实现分离。SPE从血液和尿液中回收残杀威和IPP的回收率超过85%。在大鼠血液和尿液中，残杀威的验证校准范围为0.5至100 μg/L，IPP为2至100 μg/L。血液和尿液中残杀威的定量限分别为0.5和0.8 μg/L，IPP分别为2.0和4.2 μg/L。展示了该方法在特异性、灵敏度、线性、精密度、准确度和稳定性方面的验证结果。通过对口服最低剂量残杀威的大鼠的尿液和血液进行分析，证明了该方法的适用性。
