全自动加速溶剂萃取-高效液相色谱-串联质谱法测定土壤中6种抗生素的残留量  

Determination of Residues of 6 Antibiotics in Soil by High Performance Liquid Chromatography Tandem Mass Spectrometry with Automatic Accelerated Solvent Extraction

作　　者：潘晓春 PAN Xiaochun(Shandong Ketai Environmental Monitoring Co.,Ltd.,Linyi 276007,China)

机构地区：[1]山东科泰环境监测有限公司,临沂276007

出　　处：《理化检验（化学分册）》2023年第3期337-341,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：随机选取代表性土壤样品约1 kg,四分法将土壤样品缩分,取约200 g风干、粉碎、过筛。取上述土壤样品10.0 g置于萃取池中,加入硅藻土15.0 g混合均匀后进行加速溶剂萃取(ASE),采用凝胶净化系统净化提取液。取净化液10 mL,于50℃氮吹至近干,残渣用1 mL甲醇溶解,过0.22μm滤膜,采用高效液相色谱-串联质谱法(HPLC-MS/MS)测定其中林可霉素、克林霉素、洛美沙星、培氟沙星、恩诺沙星和环丙沙星等6种抗生素的含量,质谱分析采用多反应监测模式。结果表明,6种抗生素的质量浓度在0.001~1.0 mg·L^(-1)内与对应的峰面积呈线性关系,检出限(3S/N)为0.004~0.019μg·kg^(-1)。方法用于分析单标准溶液和加标样品溶液,所得测定值的相对标准偏差(n=6)均小于4.0%。按标准加入法进行回收试验,回收率为83.8%~105%。方法用于实际样品分析,6种抗生素的检出量为15.7~221.6μg·kg^(-1)。The representative soil samples(about 1 kg)were randomly selected and divided into four parts,about 200 g of which was air dried,pulverized and sifted.10.0 g of the above soil sample was taken into the extraction pool,and 15.0 g of diatomite was added.After mixing evenly,accelerated solvent extraction(ASE)was carried out,and the extract was purified by a gel purification system.10 mL of the purified solution was taken and blown to nearly dryness at 50℃by nitrogen.The residue was dissolved in 1 mL of methanol and the solution was passed through 0.22μm filtration membrane.6 antibiotics including lincomycin,clindamycin,lomefloxacin,pefloxacin,ennofloxacin and ciprofloxacin were determined by high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS).Multiple reaction monitoring mode was used for MS analysis.As shown by the results,linear relationships between the values of corresponding peak area and mass concentration of 6 antibiotics were found in the range of 0.001^(-1).0 mg·L^(-1),with detection limits(3S/N)in the range of 0.004-0.019μg·kg^(-1).The single standard solution and the spiked sample solution were analyzed by this method,with RSDs(n=6)of the determined values less than 4.0%.Test for recovery was made by standard addition method,giving results in the range of 83.8%^(-1)05%.This method was applied to analysis of actual samples,and the detection amounts of 6 antibiotics were 15.7-221.6μg·kg^(-1).

关 键 词：全自动加速溶剂萃取(ASE) 土壤 抗生素 林可霉素 洛美沙星 高效液相色谱-串联质谱法(HPLC-MS/MS) 

分 类 号：O657.63[理学—分析化学]