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目的建立离子液体分散液相微萃取-HPLC检测血浆中溴敌隆的方法。方法以1-己基-3-甲基咪唑六氟磷酸盐([HMIM]PF6)为萃取剂,甲醇为分散剂,提取血浆中的溴敌隆,用HPLC分析其含量;考察了萃取剂和分散剂体积、样品pH值、NaCl浓度、萃取时间和离心时间等因素对萃取效率的影响。结果优化的溴敌隆分散液相微萃取操作条件为:萃取剂[HMIM]PF650μL,分散剂甲醇100μL,样品pH值5.0,萃取时间5min,离心时间8 min。方法的线性范围:0.01～5.0μg/mL,检测限:1.1 ng/mL(S/N>3)。该法低、中、高浓度的平均加标回收率分别为76.4%,82.6%,92.1%,RSD分别为4.17%,2.99%,1.67%(n=6)。结论本方法检测血浆中的溴敌隆,简便快速、准确实用,满足中毒检测及临床诊断治疗的需要。
Objective To establish a method for the determination of bromadiolone in plasma by ionic liquid dispersion liquid phase microextraction-HPLC. Methods 1-Hexyl-3-methylimidazolium hexafluorophosphate ([HMIM] PF6) was used as extractant and methanol as dispersant. The bromadiolone in plasma was extracted and its content was analyzed by HPLC. The effects of extractant and dispersant The volume of the sample, the pH value of the sample, the NaCl concentration, the extraction time and the centrifugation time on the extraction efficiency. Results The optimal conditions for the extraction of bromadiolone were as follows: extraction agent [HMIM] PF650μL, dispersant methanol 100μL, pH 5.0, extraction time 5min and centrifugation time 8min. The linear range of the method was 0.01-5.0 μg / mL with a limit of detection of 1.1 ng / mL (S / N> 3). The mean spike recoveries of low, middle and high concentrations were 76.4%, 82.6% and 92.1%, respectively, with RSDs of 4.17%, 2.99% and 1.67%, respectively (n = 6). Conclusion The method for the determination of bromadiolone in plasma is simple, rapid, accurate and practical, and meets the need of poisoning detection and clinical diagnosis and treatment.