加速溶剂萃取-固相萃取-超高效液相色谱-串联质谱法测定土壤中20种抗生素的含量  

Determination of 20 Antibiotics in Soil by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry with Accelerated Solvent Extraction and Solid Phase Extraction

作　　者：邹佳洁 刘安 秦冲 央珠 李然 刘俊妙 ZOU Jiajie;LIU An;QIN Chong;YANG Zhu;LI Ran;LIU Junmiao(Hebei Key Laboratory of Mineral Resources and Ecological Environment Monitoring,Hebei Research Center for Geoanalysis,Baoding 071051,China)

机构地区：[1]河北省地质实验测试中心河北省矿产资源与生态环境监测重点实验室,保定071051

出　　处：《理化检验（化学分册）》2024年第6期598-605,共8页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：河北省地质矿产勘查开发局科技项目(13000022P0069B410047T)。

摘　　要：提出了加速溶剂萃取-固相萃取-超高效液相色谱-串联质谱法测定土壤中(氯霉素类、喹诺酮类、磺胺类和四环素类)20种抗生素含量的方法。土壤样品经除杂、脱水、冻干、研磨和过筛后,分取2.0 g,加入4 g硅藻土和20μL 1.00 mg·L^(−1)混合内标溶液。混合物经体积比1∶1的乙腈和乙二胺四乙酸二钠(Na2EDTA)-Mcllvaine缓冲液(pH 4)的混合液加速溶剂萃取后,收集萃取液,将其酸度调至pH 3.0,过HLB固相萃取柱。用10 mL水淋洗,10 mL体积比1∶1的甲醇和乙腈混合溶液洗脱柱子。收集洗脱液,将洗脱液氮吹至近干,用10%(体积分数)甲醇溶液定容至1.0 mL,过0.22μm滤膜,滤液供超高效液相色谱-串联质谱仪分析。在色谱分析中,以Kinetex C18色谱柱为固定相,以不同体积比的0.1%(体积分数)甲酸溶液和甲醇的混合溶液为流动相进行梯度洗脱。在质谱分析中,以电喷雾离子(ESI)源电离,多反应监测(MRM)模式检测,内标法定量。结果表明:20种抗生素在质量浓度0.50~250μg·L^(−1)内与其内标质量浓度的比值和峰面积比值呈线性关系,检出限(3.143s)为0.10~0.55μg·kg−1;2.0,10.0,100μg·kg^(−1)加标浓度水平下20种抗生素的回收率为60.0%~126%,测定值的相对标准偏差(n=6)为4.0%~19%。方法用于8个实际土壤样品的分析,检出了10种抗生素,检出量为2.2~75.6μg·kg−1。The method for determination of 20 antibiotics(including chloramphenicols,quinolones,sulfonamides,and tetracyclines)in soil by ultra-high performance liquid chromatography-tandem mass spectrometry with accelerated solvent extraction and solid phase extraction.After impurity removal,dehydration,freeze-drying,grinding and sieving,2.0 g of soil sample was taken,and 4 g of diatomaceous earth and 20μL of 1.00 mg·L^(−1)mixed internal standard solution were added.The mixture was treated by accelerated solvent extraction with the mixed solution composed of acetonitrile and Na2EDTA-Mcllvaine buffer solution(pH 4)at volume ratio of 1∶1.The extraction solution was collected and its acidity was adjusted to pH 3.0 before passing through the HLB solid phase extraction column.The column was rinsed by 10 mL of water,and eluted by 10 mL of the mixed solution of methanol and acetonitrile at volume ratio of 1∶1.The eluate was collected,and blown to near dryness by nitrogen,and its volume was made up to 1.0 mL with 10%(volume fraction)methanol solution.The solution was passed through a 0.22μm filter membrane,and the filtrate was used for analysis by ultra-high performance liquid chromatograph-tandem mass spectrometer.In chromatographic analysis,the Kinetex C18 column was used as the stationary phase,and the mixed solution of 0.1%(volume fraction)formic acid solution and methanol at different volume ratios was used as the mobile phase for gradient elution.In the mass spectrometry analysis,the electrospray ionization(ESI)source was used for ionization,the multiple reaction monitoring(MRM)mode was used for detection,and the internal standard method was used for quantification.It was shown that linear relationships between values of the mass concentration ratio and the peak area ratio of 20 antibiotics to internal standards were kept in the range of 0.50-250μg·L^(−1),with detection limits(3.143s)in the range of 0.10-0.55μg·kg^(−1).At the spiked concentration levels of 2.0,10.0,100μg·kg^(−1),recoveries of 20 antibiot

关 键 词：加速溶剂萃取 固相萃取 超高效液相色谱-串联质谱法 土壤 抗生素 

分 类 号：O657.63[理学—分析化学]