【摘要】 目的:建立兔血浆中氟虫腈(Fipronil)及其代谢物砜化物(Fipronil sulfone)的高效液相色谱检测法。方法:高效液相色谱仪为Agilent 1100系列;血浆经乙醚萃取浓缩,以Hypersil ODS-C18(4.6mm×250mm,5μm)为色谱分析柱;以乙腈-甲醇-水(26:24:50,V/V/V)为流动相,流速为1.0ml·min-1;检测波长为276nm;内标为地西泮。对兔血浆中的氟虫腈及其砜化物进行检测。结果:氟虫腈及其砜化物浓度在0.05～5.00mg·L-1范围内均具有良好的线性关系(r=0.999);最低检测限均为为0.05mg·L-1;相对回收率分别为(101.08±6.13)%和(100.68±4.78)%,绝对回收率分别为(80.24%±2.58)%和(81.77±2.64)%;日内精密度变异系数分别为(5.55±1.24)%和(5.59±1.25)%;日间精密度变异系数分别为(5.91±1.44)%和(7.27±1.20)%。结论:本研究采用的反相-高效液相色谱法快速、简便、灵敏、准确,可用于兔血浆氟虫腈及其砜化物的检测和毒物代谢动力学研究。更多还原

【Abstract】 Objective:To establish a high performance liquid chromatography method for the determi-nation of Fipronil and its Metabolit(eFipronil Sulfone)in rabbit plasma. Methods: High performance liquid chromatography were equipped with Agilent 1100 series. Fipronil and Fipronil Sulfone were extracted from plasma with diethyl ether. The analytical column was packed with Hypersil ODS-C1(84.6 mm×250 mm, 5μm). The mobile phase was acetonitrile-methanol-water( 26:24:50, V/V/V) and the flow rate was 1.0 ml· min-1. The UV detection wavelength was 276 nm. The internal standard was Diazapam. Using this HPLC, the plasma Fipronil and Fipronil Sulfone concentration were determined. Results: Excellent liner relation-ship of Fipronil and Fipronil Sulfone was obtained from the range of 0.05 to 5.00 mg·L-1( r=0.999), the limit determination of Fipronil and Fipronil Sulfone was 0.05 mg·L-1. The average relative recovery of Fipronil and Fipronil Sulfone was 101.08% ±6.13% and 100.68% ±4.78%, respectively;the average absolute recovery was 80.24%±2.58% and 81.77%±2.64% respectively. The intra-day precision RSD was 5.55%±1.24% and 5.59%±1.25% and inter-day precision RSD was 5.91%±1.44% and 7.27%±1.20%, respectively. Conclusion: The method for determination of Fipronil and Fipronil Sulfone concentration in rabbits plasma and for study of toxicokinetics is simple, sensitive and accurate.更多还原