Croes K, Martens F, Desmet K
Laboratory of Emergency Toxicology, U.Z. Gasthuisberg, Leuven, Belgium.
J Anal Toxicol. 1993 Sep;17(5):310-2. doi: 10.1093/jat/17.5.310.
An HPLC method for the quantitation of paraquat in urine was applied to serum. Sample preparation consisted of ion-pair extraction on disposable cartridges of end-capped octadecyl silica. The paraquat thus extracted, was quantitated by HPLC using 1,1'-diethyl-4,4'-dipyridyl dichloride as an internal standard. Relatively small sample volumes (1 mL serum) were required. Within- and between-assay coefficients of variation for the HPLC technique were 2.9% and 4.0%, respectively, at low paraquat serum concentration (0.4 microgram/mL), and 2.4% and 3.2% at high paraquat serum concentration (4.0 micrograms/mL). The between-assay coefficient of variation for the total procedure, including the extraction, was 5.6% at low concentration (0.4 microgram/mL). Serum concentration levels down to 0.025 microgram/mL could be quantitated. The technique was checked for interference from muscle relaxants (pancuronium bromide and vecuronium bromide) and from anticoagulants (heparin and K2EDTA). No interference was observed.
一种用于尿液中百草枯定量分析的高效液相色谱（HPLC）方法被应用于血清检测。样品制备包括在封端十八烷基硅胶一次性柱上进行离子对萃取。如此萃取得到的百草枯，以1,1'-二乙基-4,4'-二吡啶二氯化物作为内标，通过HPLC进行定量分析。所需样品体积相对较小（1 mL血清）。在低百草枯血清浓度（0.4微克/毫升）时，HPLC技术的批内和批间变异系数分别为2.9%和4.0%，在高百草枯血清浓度（4.0微克/毫升）时分别为2.4%和3.2%。包括萃取在内的整个检测过程的批间变异系数在低浓度（0.4微克/毫升）时为5.6%。血清浓度低至0.025微克/毫升时仍可进行定量分析。该技术针对肌肉松弛剂（潘库溴铵和维库溴铵）及抗凝剂（肝素和乙二胺四乙酸二钾）的干扰进行了检测，未观察到干扰现象。
