摘要
针对腐败血与肝脏中毒扁豆碱、α-茄碱、α-卡茄碱以及秋水仙碱等四种食源性有毒生物碱建立QuEChERS结合超高效液相色谱-三重四级杆质谱(UPLC-MS/MS)提取检测方法。腐败血液前处理采用Φ5%甲醇-乙腈作为萃取剂,30 mg NaCl与20 mg无水MgSO4组合作为盐析剂,20 mg C18粉末作为净化剂;肝脏采用2 mL甲醇萃取,50 mg的C18、60 mg的PSA和10 mg的GCB作为净化剂。UPLC-MS/MS分析以乙腈为有机相,Φ0.1%甲酸-5 mmol·L-1甲酸铵溶液作为水相,使用电喷雾电离源,正离子电离,多反应监测模式下检测。腐败血样本中四种生物碱检测限在0.07~0.1μg·L-1,定量限在0.3~0.55μg·L-1;肝脏样本中四种生物碱检测限在0.1~1.0μg·g-1,定量限在0.3~3.0μg·g-1。该方法操作简便,灵敏度高,线性范围宽,可应用于医疗卫生、法庭科学等多个领域的腐败血中四种食源性有毒生物碱的准确、快速检测。
A QuEChERS-Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry(QuEChERS-UPLC-MS/MS)method was established for the detection of four foodborne toxic alkaloids(physostigmine,α-solanine,α-chaconine and colchicine)in the putrefied blood or liver.For the putrefied blood,5%methanol-acetonitrile was used as extractant,30 mg NaCl and 20 mg anhydrous MgSO4 as salting-out agent and 20 mg C18 powder as purificant.For the liver,acetonitrile was used as extractant,50 mg C18,60 mg PSA and10 mg GCB powder were used as purificant.In UPLC-MS/MS analysis,acetonitrile and 5 mmol·L-1 ammonium formate-0.1%formic acid-water system were used as the mobile phases,while positive electrospray ionization and MRM scan mode were used.The LODs of four alkaloids in the putrefied blood were0.07~0.1μg·L-1,and the LOQs were0.3~0.55μg·L-1.In the liver,the LODs of four alkaloids were0.1~1.0μg·g-1 and the LOQs were0.3~3.0μg·g-1.The method is simple,sensitive and has a wide linear range,which can be applied to the accurate and rapid detection of four food-borne toxic alkaloids in putrefied blood and liver in various fields such as medical and forensic science.
作者
钟世豪
任昕昕
黄健
黄健
栾玉静
于忠山
ZHONG Shi-hao;REN Xin-xin;HUANG Jian;HUANG Jian;LUAN Yu-jing;YU Zhong-shan(School of Forensic Science,People's Public Security University of China,Beijing 100038,China;Institute of Forensic Science,Ministry of Public Security,Beijing 100038,China;School of Information Technology&Network Security,People's Public Security University of China,Beijing 100038,China)
出处
《化学研究与应用》
CAS
CSCD
北大核心
2020年第7期1126-1133,共8页
Chemical Research and Application
基金
公安部技术研究计划项目(2018JSYJC10)资助
中央级公益性科研院所基本科研业务费项目(2018JB013)资助。
