Jin Mi-Cong, Ren Yi-Ping, Xu Xiao-Min, Chen Xiao-Hong
Ningbo Municipal Center for Disease Control and Prevention, Ningbo 315010, China.
Forensic Sci Int. 2007 Aug 24;171(1):52-6. doi: 10.1016/j.forsciint.2006.10.005. Epub 2006 Nov 13.
A rapid, sensitive and selective high-performance liquid chromatography tandem mass spectrometric method (HPLC/MS-MS) has been developed and validated for the determination of bromadiolone in whole blood using warfarin as an internal standard (IS). Bromadiolone was extracted from the whole blood samples by liquid-liquid extraction with ethyl acetate. Multiple-reaction monitoring (MRM) was used to detect bromadiolone and IS, using precursor --> product ion combinations at m/z 527 --> 465 and 307 --> 161, respectively. The calibration curve was linear (r2=0.998) in the concentration range of 0.5-100.0 ng/mL with a lower limit of quantification of 0.5 ng/mL in whole blood. Intra- and inter-day relative standard deviations (R.S.D.s) were less than 7.5 and 11.9%, respectively. Recoveries of bromadiolone ranged from 82.1 to 85.2%. This method is found to be determined trace bromadiolone in whole blood and can be used in the diagnosis of the poisoned human beings.
已开发并验证了一种快速、灵敏且选择性高的高效液相色谱串联质谱法（HPLC/MS-MS），以华法林作为内标（IS）来测定全血中的溴敌隆。通过用乙酸乙酯进行液液萃取从全血样品中提取溴敌隆。采用多反应监测（MRM）分别以m/z 527→465和307→161的前体离子→产物离子组合来检测溴敌隆和内标。校准曲线在0.5 - 100.0 ng/mL浓度范围内呈线性（r2 = 0.998），全血中的定量下限为0.5 ng/mL。日内和日间相对标准偏差（R.S.D.s）分别小于7.5%和11.9%。溴敌隆的回收率在82.1%至85.2%之间。该方法可用于测定全血中的痕量溴敌隆，可用于中毒人员的诊断。
