Mu Shuhe, Wang Chunyu, Liu Huan, Han Gang, Wu Lidong, Li Jincheng
Chinese Academy of Fishery Sciences, Beijing, P. R. China.
Key Laboratory of Control of Quality and Safety for Aquatic Products, Ministry of Agriculture, Beijing, P. R. China.
Biomed Chromatogr. 2021 Oct;35(10):e5176. doi: 10.1002/bmc.5176. Epub 2021 May 28.
A novelty single-step cleanup method combined with HPLC coupled with triple quadrupole-linear ion trap MS/MS (HPLC-QTRAP-MS/MS) was developed for the analysis of tricaine, tetracaine, and bupivacaine in fish tissue. The target analytes were extracted using acetonitrile based on the modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method under ultrasound irradiation. A cheap analytical filtration syringe (CAFS) cleanup column for single-step purification was proposed first; 300 mg of primary/secondary amino was proposed as the optimum purification sorbent; 1 mL of acetonitrile extract was transferred into a CAFS cleanup column and purified for analysis using HPLC-QTRAP-MS/MS. The limits of detection and the limits of quantification were 2.0 and 5.0 μg kg , respectively. The recoveries were in the range of 88.73-108.72%. Inter-day and intra-day relative standard deviations were lower than 15% for all analytes. The developed method has been applied to measure real samples obtained from the local market.
开发了一种新颖的单步净化方法，结合高效液相色谱与三重四极杆-线性离子阱串联质谱（HPLC-QTRAP-MS/MS），用于分析鱼组织中的丁卡因、丁哌卡因和布比卡因。基于改良的QuEChERS（快速、简便、廉价、有效、耐用且安全）方法，在超声辐射下使用乙腈提取目标分析物。首次提出了一种用于单步净化的廉价分析过滤注射器（CAFS）净化柱；建议使用300 mg的伯/仲氨基作为最佳净化吸附剂；将1 mL乙腈提取物转移至CAFS净化柱中，进行净化后使用HPLC-QTRAP-MS/MS进行分析。检测限和定量限分别为2.0和5.0 μg/kg。回收率在88.73%至108.72%之间。所有分析物的日间和日内相对标准偏差均低于15%。所开发的方法已应用于测量从当地市场获取的实际样品。
