Zhan Lan-fen, Liu Ming-dong, Yan You-yi, Ye Yi, Wang Wei, Wang Zhi-hui, Zhao Jun-hong, Liao Lin-chuan
West China School of Preclinical and Forensic Medicine, Sichuan University, Chengdu 610041, China.
Fa Yi Xue Za Zhi. 2012 Oct;28(5):347-50.
To establish a method for determination of strychnine and brucine in formaldehyde fixed tissue by LC-MS/MS analysis.
The samples were pretreated with solid phase extraction using SCX cartridges and separated on SB-C18 column with mobile phase 0.1% formic acid : 0.1% formic acid-acetonitrile (75:25). Electrospray ionization (ESI) source was utilized and operated in positive ion mode. Multiple reactions monitoring (MRM) mode was applied. External standard method was applied for quantitation.
The chromatographic separation of strychnine and brucine in formaldehyde fixed nephritic and hepatic tissues resulted successfully. The standard curve was linear in the range of 0.002-2.0 microg/g for strychnine and brucine in formaldehyde fixed tissues, and the correlation coefficient was more than 0.996. The limits of detection (LOD) of strychnine and brucine in nephritic tissues were 0.06ng/g and 0.03 ng/g, respectively. The LOD of both chemicals were 0.3 ng/g in hepatic tissues. The extraction recovery rate was more than 74.5%. The precision of intra-day and inter-day were both less than 8.2%.
Strychnine and brucine can be sensitive to be determined in formaldehyde fixed tissue by LC-MS/MS analysis. It can be applied in the forensic toxicological analysis.
建立一种通过液相色谱-串联质谱（LC-MS/MS）分析测定甲醛固定组织中士的宁和马钱子碱的方法。
样品采用强阳离子交换（SCX）柱进行固相萃取预处理，在SB-C18柱上分离，流动相为0.1%甲酸：0.1%甲酸-乙腈（75:25）。采用电喷雾电离（ESI）源，以正离子模式运行。应用多反应监测（MRM）模式。采用外标法进行定量。
成功实现了甲醛固定的肾组织和肝组织中士的宁和马钱子碱的色谱分离。甲醛固定组织中士的宁和马钱子碱的标准曲线在0.002 - 2.0微克/克范围内呈线性，相关系数大于0.996。肾组织中士的宁和马钱子碱的检测限（LOD）分别为0.06纳克/克和0.03纳克/克。两种化学物质在肝组织中的LOD均为0.3纳克/克。提取回收率大于74.5%。日内和日间精密度均小于8.2%。
通过LC-MS/MS分析可灵敏地测定甲醛固定组织中的士的宁和马钱子碱。该方法可应用于法医毒理学分析。
