摘要
建立了基质固相分散萃取-高效液相色谱串联质谱法(MSPD-HPLC-MS/MS)测定土壤中3种磺酰脲类除草剂(氯磺隆、甲磺隆、苯磺隆)残留的分析方法。对基于球磨的基质固相分散萃取条件进行了详细优化,最终确定最佳条件为:0.2 g土壤样品、0.8 g HC-C18粉末状分散剂与直径为8 mm的小钢珠一起球磨10 min后,转移至空的玻璃萃取小柱,用10 m L乙腈洗脱,氮气吹干后用甲醇定容至0.6 m L,再经0.22μm的滤膜抽滤后装入自动进样瓶中。用Syncronis C18反相色谱柱分离,以甲醇(A)~1‰甲酸溶液(B)为流动相进行梯度洗脱,选择反应监测(SRM)模式下进行检测。氯磺隆在20~200μg·kg^(-1),甲磺隆和苯磺隆在10~200μg·kg^(-1)范围内线性良好,相关系数r在0.997 9~0.999 5。土壤样品的平均加标回收率在84.7%~104.6%,相对标准偏差在4.5%~7.9%(n=5)。方法的检出限(S/N=3)0.32~0.68μg·kg^(-1)。该方法简单、效率高、干扰少、回收率高,满足土壤中除草剂的残留分析要求。
An analytical method for the simultaneous determination of 3 sulfonylurea herbicides（ Chloride methyl,Methyl methyl,Tribenuron） was established by matrix solid-phase dispersion extraction（ MSPD） with high performance liquid chromatography tandem mass spectrometry（ HPLC-MS / MS）. Based on ball milling of sample pretreatment of MSPD,the extraction conditions were optimized in detail as following： grinded about 0. 2 g soil sample and 0. 8 g HC-C18 solid phase extraction powder with 8 mm small steel ball for 10 min and then loaded into the empty glass extraction column. The mixture was eluted with 10 mL of acetone,and concentrated to 0. 6 mL with methanol,then choulved by the 0. 22 μm membrane and then transfered to the automatic sample bottle. The 3 sulfonylurea herbicides were separated upon a Syncronis C18 column using methanol（ A） ～ 1‰ formic acid solution（ B） as mobile phase by gradient elution,and detected by MS under selected reaction monitoring（ SRM） mode. The results indicated that the Chlorsulfuron achieved the good linearities in the range of 20 ～ 200 μg·kg^-1,and the other two sulfonylurea herbicides achieved the good linearities in the range of 10 ～200 μg·kg^-1,with correlation coefficients from 0. 997 9 ～ 0. 999 5. The recoveries at three spiked levels were ranged from 84. 7% ～ 104. 6% and RSDs were 4. 5% ～ 7. 9%. The limits of detection（ LODs） for the target compounds ranged from 0. 32 ～ 0. 68 μg·kg^-1. The suggested method was simple,efficient,and less interference with high recovery rate,and met the analytical requirements of herbicide residues in soil.
出处
《中国土壤与肥料》
CAS
CSCD
北大核心
2016年第5期148-152,共5页
Soil and Fertilizer Sciences in China
关键词
基质固相分散萃取
高效液相色谱串联质谱
磺酰脲类除草剂
土壤
matrix solid-phase dispersion
high performance liquid chromatography tandem mass spectrometry
sulfonylurea herbicide
soil
