摘要
基于高效液相色谱-四级杆-飞行时间质谱法(HPLC-Q-TOF-MSMS)技术,建立了快速筛查和分析蜂蜜中26种生物碱的方法。该方法建立了生物碱检测数据库,其中包含26种生物碱的一级精确质量数及保留时间和二级离子谱库。样品采用QuEChERS法提取,加入PSA固相萃取粉末净化,采用,ACE Excel C18-AR(4.6×150 mm,2.7μm)色谱柱进行分离,5 mmol/L甲酸铵水溶液(含0.1%甲酸)和乙腈作为流动相梯度洗脱,外标法定量。结果表明:26种生物碱在0.5~50 ng/mL的线性范围内关系良好,相关系数(r)均在0.99以上(),样品回收率在79.7%~94.3%,相对标准偏差RSD在1.54%~6.93%。检出限0.6~6.0μg/kg,定量限2.0~20μg/kg。本方法前处理操作简单、高效,为生物碱残留的快速筛查和定量检测提供了可靠的技术支持。
A method for the fast screening and detection of 26 alkaloids in honey was established based on high performance liquid chromatography-quadrupole-time of flight mass spectrometry(HPLC-Q-TOF-MSMS).The method established a database for the detection of alkaloids,which contained the exact mass numbers and retention times of 26 alkaloids at prima⁃ry level and a secondary ion spectrum library.The samples were extracted by QuEChERS method,cleaned up by adding PSA solid phase extraction powder,and separated by an ACE Excel C18-AR(4.6×150 mm,2.7μm)with aqueous solution(containing 0.1%formic acid and 5 mmol/L ammonium formate)and acetonitrile as the mobile phase.External standard method was used for quantitative analysis.The results showed that the 26 alkaloids had good linear relationships within 0.5~50 ng/mL,and the correlation coefficients(r)were all above 0.99,the sample recoveries were in the range of 79.7%~94.3%,and the relative standard deviations(RSDs)were in the range of 1.54%~6.93%.The limits of detection were 0.6~6.0μg/kg and the limits of quantification were 2.0~20μg/kg.The method is simple,efficient and provides a reliable techni⁃cal support for the rapid screening and quantitative determination of alkaloid residues.
作者
王鹭骁
袁文萱
吴娇敏
王东
方恩华
徐敦明
Wang Lu-xiao;Yuan Wen-xuan;Wu Jiao-min;Wang Dong;Fang En-hua;Xu Dun-ming*(Xiamen Customs Technical Center,Xiamen,Fujian 361013,China)
出处
《福建分析测试》
CAS
2023年第3期1-8,共8页
Fujian Analysis & Testing
基金
海关总署科技项目(2020HK223)。
