加速溶剂萃取-离子色谱-串联质谱法测定种植土壤中5种强极性农药的残留量  

Determination of Residues of 5 Strong Polar Pesticides in Planting Soil by Ion Chromatography-Tandem Mass Spectrometry with Accelerated Solvent Extraction

作　　者：李海侠 李丽萍 丁可 LI Haixia;LI Liping;DING Ke(Linyi Ecological Environment Monitoring Center of Shandong Province,Linyi 276000,China)

机构地区：[1]山东省临沂生态环境监测中心,临沂276000

出　　处：《理化检验（化学分册）》2024年第8期827-831,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：考虑到采用现有方法检测草铵膦、增甘膦、脱落酸、灭草松和氨甲基膦酸时存在需要衍生化处理、色谱保留时间短等问题,进行了题示研究。取种植土壤样品,除杂、风干、过筛后,分取10 g,加入硅藻土20 g和体积比2∶1的甲醇-丙酮混合溶液25 mL进行加速溶剂萃取。提取液过0.22μm聚醚砜滤膜,弃去初滤液,取续滤液上离子色谱-串联质谱仪检测。在色谱分析中,在Dionex IonPac AS17色谱柱上以0.1 mol·L^(-1)氢氧化钠溶液淋洗分离上述5种农药;在质谱分析中,以电喷雾离子源负离子模式电离,多反应监测(MRM)模式采集数据,外标法定量。结果显示,5种农药的质量浓度在0.001~5.0 mg·L^(-1)内和峰面积呈线性关系,检出限(3S/N)分别为0.012,0.009,0.007,0.013,0.005 ng·L^(-1);3个加标浓度水平下5种农药的回收率为84.4%~103%,测定值的相对标准偏差(n=5)为1.5%~3.7%。Considering the issues of requiring derivatization processing and short chromatographic retention time on the existing methods for detection of glufosinate ammonium,glyphosine,abscisic acid,bentazone and(aminomethyl)phosphonic acid,the study mentioned by the title was conducted.The planting soil sample was taken,removed from impurities,dried by air,and sieved.An aliquot(10 g)was taken and mixed with 20 g of diatomaceous earth and 25 mL of methanol-acetone mixed solution at volume ratio of 2∶1 for accelerate solvent extraction.The extraction solution was passed through a 0.22μm polyethersulfone filter membrane,the initial filtrate was discarded,and the subsequent filtrate was detected by ion chromatograph-tandem mass spectrometer.In chromatographic analysis,0.1 mol·L^(-1)sodium hydroxide solution was used for washing and separating the above 5 pesticides on the Dionex IonPac AS17 column.In mass spectrometry analysis,the negative ion mode of the electrospray ion source was used for ionization,multiple reaction monitoring(MRM)mode was used to collect data,and external standard method was used for quantification.It was shown that linear relationships between values of the mass concentration and the peak area of the 5 pesticides were kept in the range of 0.001-5.0 mg·L^(-1),with detection limits(3S/N)of 0.012,0.009,0.007,0.013,0.005 ng·L^(-1),respectively.Recoveries of the 5 pesticides at three spiked concentration levels were found in the range of 84.4%-103%,giving RSDs(n=5)of the determined values in the range of 1.5%-3.7%.

关 键 词：加速溶剂萃取 离子色谱-串联质谱法 种植土壤 强极性农药 

分 类 号：O657.63[理学—分析化学]