分散液相微萃取-气相色谱-质谱法测定环境水样中5种芳香胺的含量
Determination of 5 Aromatic Amines in Environmental Water Sample by GC-MS with Dispersive Liquid-Liquid Microextraction
摘 要
向5 mL水样中加入0.1 g NaCl，溶解后加入50 μL三氯甲烷（萃取剂）和300 μL丙酮（分散剂），以4 000 r·min-1的转速离心2 min。采用气相色谱-质谱法测定所得有机相中5种芳香胺的含量，以内标法定量。结果表明：5种芳香胺的质量浓度在一定范围内与其峰面积与内标的峰面积的比值呈线性关系，检出限（3S/N）为0.000 1~0.001 5 mg·L-1。以实际空白水样为基体进行加标回收试验，回收率为94.7%~106%，测定值的相对标准偏差（n=6）均小于5.0%。
分散液相微萃取
芳香胺
环境水样
内标法
GC-MS
dispersive liquid-liquid microextraction
aromatic amine
environmental water sample
internal standard
Abstract
0.1 g of NaCl was added into 5 mL of water sample, and after dissolving, 50 μL of trichloromethane as extractant and 300 μL of acetone as dispersant were added and the mixture was centrifuged at a rotating speed of 4 000 r·min-1 for 2 min. The 5 aromatic amines in the organic phase were determined by GC-MS, and the internal standard method was used for quantitative analysis. As shown by the results, linear relationships between the ratios of peak areas of 5 aromatic amines to peak areas of the internal standard and the mass concentration of 5 aromatic amines were found in definite ranges, with detection limits (3S/N) in the range of 0.000 1-0.001 5 mg·L-1. Test for recovery was made by standard addition method on the base of actual blank water, giving results in the range of 94.7%-106%, and RSDs (n=6) were less than 5.0%.
中图分类号 O652.63 DOI 10.11973/lhjy-hx201810011
所属栏目 工作简报
基金项目 江苏省高校自然科学基金面上项目（16KJB150016）；南京大学金陵学院教学改革项目（0010521611）；江苏省自然科学基金项目（BK20131343）
收稿日期 2017/10/17
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备注丁明珍,讲师,主要从事色谱及色谱-质谱联用在食品、药品和环境分析应用方面的研究
引用该论文: DING Mingzhen,PENG Jing,MA Shaoling,JIANG Yong,QIN Wenjing. Determination of 5 Aromatic Amines in Environmental Water Sample by GC-MS with Dispersive Liquid-Liquid Microextraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(10): 1172～1176
丁明珍,彭璟,马少玲,姜勇,秦文璟. 分散液相微萃取-气相色谱-质谱法测定环境水样中5种芳香胺的含量[J]. 理化检验－化学分册, 2018, 54(10): 1172～1176
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【3】周文敏,傅德黔,孙宗光.中国水中优先控制污染物黑名单的确定[J].环境科学研究, 1991,4(6):9-12.
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【6】储燕萍,唐莺,韩英,等.气相色谱/质谱联用法测定饮用水源水中苯胺类化合物[J].环境监测管理与技术, 2011,23(5):58-61.
【7】林忠胜,马新东,周传光.气相色谱/质谱法测定海水中芳香胺[J].分析试验室, 2009,28(5):11-13.
【8】HADJMOHAMMADI M R, EBRAHIMI S, NAZARI S S S J. Determination of aromatic amines in environmental water samples using solid-phase extraction modified with sodium dodecyl sulphate and micellar liquid chromatography[J]. International Journal of Environmental Analytical Chemistry, 2016,96(5):1-15.
【9】ABBASI V, SARAFRAZ-YAZDI A, AMIRI A, et al. Determination of aromatic amines using solid-phase microextraction based on an ionic liquid-mediated solgel technique[J]. Journal of Chromatographic Science, 2016,54(4):677-681.
【10】陈烨,王超,许秀艳,等.顶空固相微萃取/气相色谱法快速测定水中氯代苯胺类残留[J].分析测试学报, 2014,33(9):1056-1061.
【11】胡庆兰,郑平,段连生.顶空固相微萃取-气相色谱法测定水中芳香胺类化合物[J].华中师范大学学报(自然科学版), 2012,46(4):452-455.
【12】冯文,朱莹,欧阳钢锋.超声辅助-高分子表面活性剂增强乳化微萃取测定水中多种痕量芳香胺[J].分析化学, 2015,43(7):957-963.
【13】张红医,张志军,王子川,等.盐加速沉降-分散液液微萃取-毛细管区带电泳测定水中芳香胺类化合物[J].分析化学, 2013,41(12):1875-1880.
【14】肖婷婷,诸寅,蔡强,等.在线中空纤维膜液相微萃取/高效液相色谱法测定3种痕量芳香胺[J].分析测试学报, 2015,34(10):1142-1146.
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