固相萃取-超高效液相色谱法测定土壤中土霉素、四环素及金霉素

Determination of oxytetracyline,tetracyline and chlortetracyline in soil by ultra high performance liquid chromatography with solid phase extraction

建立土壤中土霉素、四环素、金霉素残留量检测的固相萃取-超高效液相色谱法。向样品中加入Na_(2)EDTA-Mcllvaine-甲醇提取液,振荡离心后,上清液过HLB固相萃取柱净化富集。采用Agilent C_(18)色谱柱(250 mm×4.6 mm,4.6μm),以甲醇-乙腈-0.01 mol/L草酸溶液(体积比为8∶8∶84)为流动相,梯度洗脱,流量为1.0 mL/min,柱温为30℃,检测波长为355 nm。土霉素、四环素、金霉素的质量浓度在0.1~20.0μg/mL范围内与对应的色谱峰面积线性关系良好,检出限分别为0.54、0.66、0.83 mg/kg,测定结果的相对标准偏差为0.75%~4.99%(n=6),加标回收率为71.7%~97.3%。该方法可用于检测土壤中土霉素、四环素、金霉素的残留量。

A method was established for determining oxytetracycline,oxytetracycline and chlortetracycline in soil by solid phase extraction and ultra high performance liquid chromatography.Na_(2)EDTA-Mcllvaine-methanol extract was added to the sample,and the supernatant was purified and enriched by HLB solid phase extraction column after concussion centrifugation.Agilent C_(18) column(250 mm×4.6 mm,4.6μm)was used and methanol-acetonitrile-0.01 mol/L oxalic acid solution(volume ratio was 8∶8∶84)was used as the mobile phase with gradient elution,the flow rate was 1.0 mL/min,the column temperature was 30℃,and the detection wavelength was 355 nm.The linear relationship between the mass concentration of the three antibiotics and the chromatographic peak area was good in the range of 0.1-20.0μg/mL.The detection limit was 0.54,0.66 and 0.83 mg/kg,respectively.The relative standard deviation of the detection results was 0.75%-4.99%(n=6),and the recovery of standard addition was 71.7%-97.3%.This method can be used to detect the residues of oxytetracycline,tetracycline and chlortetracycline in soil.