摘要
为建立血浆样品中三氯苯达唑(TCBZ)及其代谢产物三氯苯达唑砜(TCBZSO2)和三氯苯达唑亚砜(TCBZSO)的高效液相色谱同步检测方法,以甲苯咪唑(MBZ)为内标物,将加有目标物标准品的新鲜绵羊血浆样品经甲醇提取净化和氮气浓缩等前处理后,供HPLC检测;并对以上3种目标物紫外检测方法的专属性、稳定性、准确度和灵敏度等进行了系统研究。结果表明,三氯苯达唑、三氯苯达唑砜、三氯苯达唑亚砜以及内标物甲苯咪唑的保留时间分别为10.021、4.373、5.407、3.420min,分离良好,且不受干扰峰的影响;目标物均在0.05μg/mL～6.4μg/mL范围内呈现良好的线性关系,R2分别为0.999 5、0.999 0和0.999 1;血浆样品被测物含量的日内和日间变异系数(CV)分别小于1%和12%;绝对回收率分别为84.96%、83.84%和86.27%,内标物甲苯咪唑的绝对回收率为90.16%;最低检测限为0.05μg/mL。表明该方法适用于跟踪检测三氯苯达唑及其代谢产物在绵羊血浆中的浓度,是一种稳定而准确的检测方法。
This study was designed to develop a method for simultaneous determination of triclabendazole （TCBZ） and its metabolites sulphone （TCBZSOz）, sulphoxide （TCBZSO）by high-performance liquid chromatography （HPLC） with ultraviolet detector. Mebendazole （MBZ） was used as internal standard. The plasma samples including standard triclabendazole and its metabolites were extracted by methanol, concentrated by nitrogen and injected into the HPLC system for analysis. The specificity, stability, accuracy and sensitivity of the method was evaluated systematically. The results showed that the retention time of TCBZ, TCBZSO2, TCBZSO and mebendazole（internal standard） are 10. 021 rain,4. 373 rain,5. 407 min and 3. 420 min,respectively, and they can be separated well without any interference. The concentration of triclabendazole and its metabolites were showed a good linear relationship in the range of 0.05 g/mL-6.4 /g/mL, with correlation coefficients （R2） of 0.＂ 999 5, 0. 999 0 and 0. 999 1, respectively, the intraday and interday coefficients of variation （CV） were respectively less than 1% and 12%, the relative recovery were 84.96%, 83.84%, 86.27% and 90. 16% （internal standard）, the limit of detection was 0.05 /g/mL. Therefore, the established method was one of the stable, accurate and suitable methods for tracking the trace concentration of triclabendazole and its metabolites in sheep plasma.
出处
《动物医学进展》
CSCD
北大核心
2013年第4期60-64,共5页
Progress In Veterinary Medicine
基金
内蒙古自然科学基金项目(2010MS0404)
关键词
三氯苯达唑
三氯苯达唑砜
三氯苯达唑亚砜
高效液相色谱紫外检测法
绵羊血浆
triclabendazole
triclabendazole sulphone
triclabendazole sulphoxide
high-performance liquidchromatography （HPLC） with ultraviolet detector ~ sheep plasma
