| 预衍生化-气相色谱-质谱法测定水中酸性除草剂 |
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| 引用本文： | 张莉,桂建业,张永涛,左海英,李小亚,张桂芹. 预衍生化-气相色谱-质谱法测定水中酸性除草剂[J]. 理化检验(化学分册), 2011, 0(1) |
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| 作者姓名： | 张莉 桂建业 张永涛 左海英 李小亚 张桂芹 |
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| 作者单位： | 中国地质科学院水文地质环境地质研究所;西南大学外国语学院; |
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| 基金项目： | 中国地质科学院水文地质环境地质研究所基本科研业务费(SK07001SK201008) |
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| 摘 要： | 向水样中逐滴加硫酸(1+2)调节至pH<2,用二氯甲烷先后提取3次。合并的提取液用无水酸性硫酸钠脱水,并蒸缩至约1 mL后用吹氮法蒸干。加入丙酮溶解残渣后,在催化剂碳酸钾存在下用五氟苄基溴进行衍生化,溶于正己烷中的衍生产物用极性硅胶柱进行纯化。先用甲苯-正己烷(1+6)混合溶剂淋洗净化柱以除去衍生产物中的干扰副产物,然后用甲苯-正己烷(9+1)从净化柱上将目标化合物洗脱,所得洗脱液经浓缩并加入八氟联苯作内标后供气相色谱-质谱分析。气相色谱中用HP-5MS毛细管色谱柱进行分离,质谱分析中用负化学离子源及选择离子扫描(SIM)。此方法对测定的14种酸性除草剂的检出限(3S/N)均小于10 ng.L-1。对所述14种除草剂做了回收试验,结果在66.0%~117.0%之间,测定7次的相对标准偏差均小于9%。
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| 关 键 词： | 气相色谱-质谱联用法 酸性除草剂 水样 预衍生化 |
GC-MS Determination of Acidic Herbicides in Water with Prederivatization |
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| ZHANG Li,GUI Jian-ye,ZHANG Yong-tao,ZUO Hai-ying,LI Xiao-ya,ZHANG Gui-qin. GC-MS Determination of Acidic Herbicides in Water with Prederivatization[J]. Physical Testing and Chemical Analysis Part B:Chemical Analgsis, 2011, 0(1) |
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| Authors: | ZHANG Li GUI Jian-ye ZHANG Yong-tao ZUO Hai-ying LI Xiao-ya ZHANG Gui-qin |
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| Affiliation: | ZHANG Li1,GUI Jian-ye1,ZHANG Yong-tao1,ZUO Hai-ying1,LI Xiao-ya1,ZHANG Gui-qin2(1.Research Institute of Hydrogeology and Environmental Geology,China Academy of Geology,Zhengding 050803,China,2.College of Foreign Language,Southwest University,Chongqing 400715,China) |
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| Abstract: | Water sample was adjusted to pH<2 by adding H2SO4(1+2) dropwise and extracted for 3 times with dichloromethane.The extracts were combined,dehydrated with anhydrous acidic sodium sulfate,concentrated to 1 mL and evaporated to near dryness by N2-blowing.The residue was taken up with acetone and derivatized with pentafluorobenzyl bromide with K2CO3 as catalyst.The derivatized product in n-hexane solution was purified on polar silica gel column.Interfering by products were removed by elution with mixture of tol... |
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| Keywords: | GC-MS Acidic herbicides Water sample Prederivatization |
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