大豆中硝磺草酮的残留量测定 |
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引用本文: | 王晓环,康頔,王德飘,吴玉娥,曾松,张侃侃,胡德禹.大豆中硝磺草酮的残留量测定[J].贵州大学学报(农业与生物科学版),2016(1):29-33. |
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作者姓名: | 王晓环 康頔 王德飘 吴玉娥 曾松 张侃侃 胡德禹 |
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作者单位: | 贵州大学 精细化工研究开发中心,贵州 贵阳,550025 |
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基金项目: | 公益性行业(农业)科研专项(201203022);贵州省重大科技专项项目(黔科合重大专项字[2013]6024号);贵州大学研究生创新基金项目(研理工2015052)。 |
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摘 要: | 为快速检测大豆中硝磺草酮残留量建立了高效液相色谱–串联质谱的新方法。大豆样品采用乙腈提取,Na Cl盐析,十八(烷)基硅烷(C_(18))和石墨化炭黑(GCB)分散固相萃取净化,以phenomenex Luna 3u C_(18)(2)100A柱为分离柱,用乙腈和0.1%氨水溶液进行梯度洗脱,电喷雾负离子(ESI~–)多反应监测,高效液相色谱–串联质谱(HPLC–MS/MS)测定。本方法条件下,硝磺草酮在0.0075–0.75μg/m L浓度范围内呈良好的线性关系(R~20.997),方法检出限(LOD)和定量限(LOQ)分别为0.0009和0.003 mg/kg。在0.003、0.03和0.3 mg/kg添加水平下,硝磺草酮的日内平均回收率为83.84–96.24%,日内相对标准偏差(RSD)为1.99–3.78%,日间平均回收率为85.13–95.25%,日间RSD为2.11–3.47%,能满足大豆中硝磺草酮检测的要求。
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关 键 词: | 硝磺草酮 大豆 QuEChERS法 高效液相色谱-串联质谱法 |
A novel QuEChERSmethod to determine the mesotrioneresidue in soybean |
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Abstract: | A novel QuEChERS method was developed for the rapid determination of mesotrione residue in soybean using high performance liquid chromatography tandem-mass spectrometry ( HPLC–MS/MS) . The samples were extracted with acetonitrile, then salted out with NaCl, purified with GCB and Cl8, separated on a phenomenex Luna 3u C18 (2) 100A column with gradient elution by using acetonitrile and 0.1% ammonia aqueous as eluant, and detected by HPLC–MS/MS under negative electrospray ionization ( ESI–) and multiple-reaction monitoring ( MRM) models. Under these condi﹣tions, mesotrione showed a good linear relationship ( R 2>0.997) in the concentration range of 0.0075–0.75 μg/mL, and the limit of quantification (LOQ) and limit of detection (LOD) in soybean were 0.003 and 0.0009 mg/kg, respec﹣tively. Three spiked levels at 0.003, 0.03 and 0.3 mg/kg were investigated, and the intra-day average recoveries ranged from 83.84% to 96.24%, with intra-day relative standard deviations ( RSDs) of 1.99-3.78%, the inter-day average re﹣coveries ranged from 85.13% to 95.25%,inter-day RSDs of 2.11-3.47%, which met the requirement of mesotrione de﹣termination in soybean. |
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Keywords: | Mesotrione Soybean QuEChERS ( Quick Easy Cheap Effective Rugged and Safe) High perform﹣ance liquid chromatography-tandem mass spectrometry |
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