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液相色谱-串联质谱法测定甘蔗中10种除草剂的残留量 被引量:10

LC-MS/MS Determination of Residual Amounts of 10 Herbicides in Sugarcane
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摘要 甘蔗样品(2.00g)用乙腈10.0mL匀质提取,提取液经QuEchERS方法净化。所得净化液进行液相分离,以Hypersil Gold色谱柱为分离柱,以不同体积比的含0.1%(体积分数)甲酸的10mmol·L^(-1)乙酸铵溶液和乙腈的混合液为流动相进行梯度洗脱,质谱分析中采用电喷雾正离子源选择反应监测模式检测。10种除草剂的质量浓度均在10~1 000μg·L^(-1)内与其对应的峰面积呈线性关系,方法的测定下限(10S/N)在2~10μg·kg^(-1)之间。以空白样品为基体进行加标回收试验,所得回收率在82.3%~120%之间,测定值的相对标准偏差(n=6)在3.9%~8.2%之间。 The pretreated sugarcane sample (2.00 g) was homogeneously extracted with 10. 0 mL acetonitrile and purified by QuEchERS method. In LC separation Hypersil Gold chromatographic column was used as stationary phase, and mixtures of 10 mmol·L^-1 ammonium acetate solution containing 0. 1% (φ) formic acid and acetonitrile mixed in different ratio were used as mobile phase in gradient elution. ESI+ and selective reaction monitoring were adopted in MS/MS. Linear relationships between values of peak area and mass concentration of the l0 herbicides were kept in the same range of 10-1 000μg·kg^-1 , with lower limits of determination (10S/N) in the range of 2- 10μg·kg^-1. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 82. 3%-120%, with RSDs (n=6) in the range of 3. 9%-8. 2%.
出处 《理化检验(化学分册)》 CSCD 北大核心 2017年第5期507-511,共5页 Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金 广西壮族自治区直属公益性科研院所基本科研业务费专项课题(2013AC206)
关键词 液相色谱-串联质谱法 甘蔗 除草剂 LC-MS/MS sugarcane herbicides
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