超高效液相色谱串联四级杆飞行时间质谱法快速测定草乌中毒患者血清中的乌头类生物碱及其代谢产物

Rapid determination of aconitoid alkaloids and their metabolites in blood serum samples of patients with aconitum poisoning by ultra performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry

中文关键词:  乌头类生物碱  超高效液相色谱串联四级杆飞行时间质谱  血清

英文关键词:aconitine alkaloids  ultra performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry  blood serum

中文摘要:

      目的 建立超高效液相色谱串联四级杆飞行时间质谱法快速检测草乌中毒者血清中乌头类生物碱及其代谢产物。方法 血样经离心后, 取0.2 mL血清用甲醇定容至2.0 mL, 涡旋混匀过滤膜后, 对草乌中毒者血样中14种乌头类生物碱及其代谢产物进行定性定量检测。结果 14种乌头类生物碱及其代谢产物在1.0~100 ng/mL的浓度范围内线性关系良好, 相关系数均大于0.99, 加标回收率为80.2%~111.9%, 相对标准偏差为0.5~3.3%。11个草乌中毒者血清中含有苯甲酰新乌头原碱, 含量约为2.11~2.38 mg/kg, 部分血清样品中还检测到滇乌头碱、印乌头碱, 含量分别为3.16~3.30 mg/kg、1.09~1.15 mg/kg。结论 该方法灵敏, 准确, 适用于血清中乌头类化合物的检测。

英文摘要:

      Objective To establish a method for rapid determination of aconitine alkaloids and their metabolites in blood serum samples of patients with aconitum poisoning by ultra performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry. Methods After centrifugation of the blood samples, 0.2 mL of blood serum were adjusted to 2.0 mL with methanol. After vortex blending and filtering membrane, 14 kinds of aconitum alkaloids and their metabolites in the blood samples of drug poisoning patients were quantitatively and qualitatively tested. Results The 14 aconitine alkaloids and their metabolites had good linear relationship in the concentration range of 1.0~100 ng/mL, the correlation coefficient was greater than 0.99, the recoveries were 80.2%?111.9%, and the relative standard deviations were 0.5%?3.3%. The blood serum of 11 blood samples of patients with aconitum poisoning had Benzoylmesaconine, the content was about 2.11?2.38 mg /kg, and aconitine and aconitine were also detected in some serum samples, the content was 3.16?3.30 mg/kg, 1.09?1.15 mg/kg respectively. Conclusion The method is sensitive, accurate and suitable for the detection of aconitum compounds in blood serum.