摘要
提出了全自动QuEChERS净化-高效液相色谱-串联质谱法(HPLC-MS/MS)测定作物土壤中春雷霉素、多抗霉素、布拉叶斯等3种抗菌素类杀菌剂残留量的方法。将作物土壤样品用粉碎机粉碎,于-18℃储存。取25 g处理后的作物土壤样品,置于QuEChERS自动样品制备系统配备的样品管中,分别加入1粒陶瓷均质子、20 mL 85%(体积分数)甲醇溶液、QuEChERS提取包、内置管(含净化剂),以转速2 000 r·min^(-1)振荡5 min,以转速6 000 r·min^(-1)离心5 min。移取2 mL净化液置于试管中,于50℃氮吹至近干,加入1 mL甲醇复溶,过0.22μm滤膜,采用HPLC-MS/MS测定滤液中3种抗菌素类杀菌剂的含量。以Waters BEH ODS C_(18)色谱柱为固定相,以不同体积比的0.1%(体积分数)甲酸溶液-乙腈混合液为流动相进行梯度洗脱,质谱分析采用电喷雾离子(ESI)源,在正离子(ESI^(+))扫描模式下进行多反应监测(MRM)模式分析。结果表明,3种抗菌素类杀菌剂的质量浓度在0.005~0.5 mg·L^(-1)内与对应的定量离子响应值呈线性关系,检出限(3S/N)为0.10~0.13μg·kg^(-1)。按照标准加入法进行回收试验,回收率为83.2%~106%,测定值的相对标准偏差(n=6)均小于5.0%。方法用于测定实际作物土壤中3种抗菌素类杀菌剂的残留量,检出量为10.11~59.07μg·kg^(-1)。
A method for determination of residues of 3 antimicrobial fungicides in crop soil,including chunlei mycin,multi anti mycin,and blades,was proposed by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)with fully automatic QuEChERS purification.The crop soil samples were crushed by a grinder,and stored at-18 ℃.25 g of the processed crop soil sample was taken,and placed in the sample tube equipped with the QuEChERS automatic sample preparation system.One ceramic homogeneous proton,20 mL of 85%(volume fraction) methanol solution,QuEChERS extraction kit,and internal tube(containing purification agent) were added respectively.The mixture was shaken at a rotational speed of 2 000 r · min^(-1) for 5 min,and centrifuged at a rotational speed of 6 000 r · min^(-1) for 5 min.2 mL of purified solution was transfered into a test tube,and blown to near dryness by nitrogen at 50 ℃,and 1 mL of methanol was added for reconstitution.The solution was passed through a 0.22 μm filter membrane,and 3 antimicrobial fungicides in the filtrate were determined by HPLC-MS/MS.Waters BEH ODS C_(18) column was usede as the stationary phase and the mixed solution composed of 0.1%(volume fraction) formic acid solution and acetonitrile at different volume ratios was used as the mobile phase for gradient elution.Electrospray ion(ESI) source was used for mass spectrometry.The targets were analyzed by multiple reaction monitoring(MRM) mode in positive ion(ESI+)scanning mode.As shown by the results,linear relationships between the corresponding quantitative ion response values and mass concentrations of 3 antimicrobial fungicides were found within 0.005-0.5 mg · L^(-1),with detection limits(3S/N) in the range of 0.10-0.13 μg · kg^(-1).Test for recovery was made by the standard addition method,giving results in the range of 83.2%-106%,with RSDs(n=6) of the determined values less than 5.0%.This method could be used to determine the residues of 3 antimicrobial fungicides in actual crop soils,and the detection amounts were in the range of 10.11-59.07 μg · kg^(-1).
作者
郑赛刚
ZHENG Saigang(Henan Nanyang Ecological Environment Monitoring Center,Nanyang 473000,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2024年第9期885-889,共5页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
