Draffan G H, Clare R A, Davies D L, Hawksworth G, Murray S, Davies D S
J Chromatogr. 1977 Sep 21;139(2):311-20. doi: 10.1016/s0021-9673(00)89326-7.
The gas chromatographic (GC) determination of the herbicide paraquat, the 1,1'-dimethyl-4,4'-dipyridyl cation in human plasma is described. In poisoning cases, plasma concentrations provide a necessary index of the severity of intoxication and a means of monitoring subsequent therapy. The methods may be extended to the specific trace analysis of paraquat in body fluids of post-mortem tissue. Reduction of fully ionised paraquat salts with sodium borohydride yields a hexahydro derivative, a diene, amenable to solvent extraction and GC. Employing 1,1'-diethyl-4,4'-dipyridyl dichloride as the internal standard, plasma concentrations of 0.1 microgram/ml (+/- 6% S.D.) may be determined with flame ionisation detection and 0.025 microgram/ml with nitrogen-selective flame ionisation. Further enhancement of specificity is achieved using selected ion monitoring mass spectrometry and the value of this technique in forensic analysis is illustrated.
本文描述了用气相色谱法（GC）测定人体血浆中除草剂百草枯（即1,1'-二甲基-4,4'-联吡啶阳离子）的方法。在中毒病例中，血浆浓度是中毒严重程度的必要指标，也是监测后续治疗的一种手段。这些方法可扩展到对死后组织体液中百草枯的特定痕量分析。用硼氢化钠还原完全电离的百草枯盐会生成一种六氢衍生物，即一种二烯，可进行溶剂萃取和气相色谱分析。以1,1'-二乙基-4,4'-联吡啶二氯化物作为内标，采用火焰离子化检测可测定血浆浓度为0.1微克/毫升（±6%标准差），采用氮选择性火焰离子化可测定血浆浓度为0.025微克/毫升。使用选择离子监测质谱法可进一步提高特异性，并说明了该技术在法医分析中的价值。
