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首页> 《中国测试》期刊 >本期导读>气相色谱质谱法测定土壤中5种苯并咪唑类的残留

气相色谱质谱法测定土壤中5种苯并咪唑类的残留

145    2021-09-23

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作者:郭延萍, 刘永玲

作者单位:海东市生态环境局,青海 海东 810600


关键词:加速溶剂萃取;气相色谱三重四级杆串联质谱;苯并咪唑类;典型土壤


摘要:

实验开发一种加速溶剂提取典型土壤中5种苯并咪唑类杀菌剂(噻菌灵、恶咪唑、抑霉唑、咪鲜胺和氟菌唑),QuEChERS (Quick、Easy、Cheap、Effective、Rugged、Safe)净化,GC-MS/MS仪定量测定的分析方法。取研细过筛后的典型土壤样品12 g装填至22 mL的萃取罐中,用乙腈-丙酮(体积比为1∶1)作为萃取溶液在加速溶剂萃取仪进行萃取;萃取液浓缩至近干,用20 mL冰醋酸(1%)-乙腈溶液转移至50 mL塑料离心管中,加入PSA净化。净化液氮吹至近干,残渣加甲醇1 mL溶解,混匀,上GC-MS/MS仪定量测定。噻菌灵、恶咪唑、抑霉唑、咪鲜胺和氟菌唑在0.05~15.0 μg/mL范围内,具有良好的线性,5种杀菌剂检测限在0.0032~0.0080 mg/kg范围内;3水平浓度加标回收率在85.9%~103.1%之间;重复性RSD(n=6)分别为3.26%、3.18%、3.75%、4.43%和2.73%。实验证明,方法具有简单、快速、重复性好、准确度高等特点,适用于典型土壤中苯并咪唑类杀菌剂残留的监测。


Determination of five benzimidazole residues in soil by gas chromatography mass spectrometry
GUO Yanping, LIU Yongling
Haidong Municipal Ecological Environment Bureau, Haidong 810600, China
Abstract: To explore accelerated solvent extraction and QuEChERS purification of 5 benzimidazoles residuals (probenazole, oxpoconazole, imazalil, prochloraz and triflumizole) in soil on gas chromatography-triple quadruplerodmass spectrometry (GC-MS/MS). Random soil samples was grinded and sifted first, then 12 g samples was took to 22 mL extraction tank. Samples were extracted on accelerate solvent extractor by acetontrile-acetone(VV, 1∶1). The extracted solution was condensed to near dry, 20 mL glacial acetic acid (1%) - acetonitrile was added to dissolve the residue, and purified by PSA. The purified solution was flowed to near dry by nitrogen, residues was volumned to 1 mL by methanol and detected on GC-MS/MS. Probenazole, oxpoconazole, imazalil, prochloraz and triflumizole showed good linear relationships in the concentration range 0.05-15.0 µg/mL. The detection limits were in the range

0.0032

-

0.0080

mg/kg and average recoveries in 3 different concentration levelswere ranged from 85.9%-103.1%. Relative standard deviation (RSD) of repeatability(n=6) were 3.26%, 3.18%, 3.75%, 4.43% and 2.73%, respectively. The results show that the method is simple, rapid, reproducible and accurate, which is suitable for the monitoring of benzimidazole fungicide residues in typical soil.
Keywords: ASE;GC-MS/MS;benzimidazoles;typical soil
2021, 47(9):82-86  收稿日期: 2020-07-03;收到修改稿日期: 2020-09-19
基金项目:
作者简介: 郭延萍(1987-),女,青海海东市人,工程师,硕士,主要从事环境监测工作
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