水中3种苯胺类混合标准样品的研究初探
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摘要
探索了水中苯胺、对硝基苯胺和间硝基苯胺多组分混合标准样品的制备技术。实验从制备介质、参比波长、流动相、稳定剂、保存条件等方面进行探索,结果表明,采用"重组法"制备水中3种苯胺类混合标准样品在SDB-C18型液相色谱柱、甲醇-水混合溶液为流动相的液相色谱仪上分离度良好。分层随机抽取10瓶样品进行瓶间均匀性检验,经单因素方差分析法统计,证明样品均匀性良好。将室温避光和4℃冷藏避光保存的样品进行稳定性检验,经趋势分析法计算,其线性直线的斜率均不显著,表明在180 d的监测期内,室温避光和4℃冷藏避光保存条件下的样品稳定性均良好,为后续开展水中有机物标准样品的研制提供了参考。
The preparation method of anilines in water reference material was introduced,including aniline,p-nitroaniline and mnitroaniline.It was prepared by the method of a spiking solution added to water,and factors in the process of preparation were investigated,such as preparation medium,reference wavelength,mobile phase,stabilizer,preservation conditions and so on. The result showed that anilines in water had a good resolution on the liquid chromatograph with SDB-C18 column,using methanol and water as mobile phase.10 Units selected by random stratified sampling coving the whole batch were obtained for homogeneity,and indicated good homogeneity using one-way analysis of variance.At ambient and 4 ℃ refrigeration storage conditions,the concentration of anilines did not change during monitoring period of 180 d.At the same time,trend analysis method was used for the stability data,and its linear slope was not significant,indicating good stability.This method provides reference for the subsequent development of organic compounds in water reference material.
The preparation method of anilines in water reference material was introduced,including aniline,p-nitroaniline and mnitroaniline.It was prepared by the method of a spiking solution added to water,and factors in the process of preparation were investigated,such as preparation medium,reference wavelength,mobile phase,stabilizer,preservation conditions and so on. The result showed that anilines in water had a good resolution on the liquid chromatograph with SDB-C18 column,using methanol and water as mobile phase.10 Units selected by random stratified sampling coving the whole batch were obtained for homogeneity,and indicated good homogeneity using one-way analysis of variance.At ambient and 4 ℃ refrigeration storage conditions,the concentration of anilines did not change during monitoring period of 180 d.At the same time,trend analysis method was used for the stability data,and its linear slope was not significant,indicating good stability.This method provides reference for the subsequent development of organic compounds in water reference material.
引文
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[4]赵云芝,谢振伟,潘乐丹,等.固相萃取/液相色谱-串联质谱法测定水中苯胺类化合物及基质干扰的消除[J].色谱,2016,34(2):289-298.
[5]周琛,骆春迎,余辉菊,等.直接进样-液相色谱-串联质谱法同时测定水中的5种苯胺类化合物[J].分析化学,2016,44(6):935-941.
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[8]鲁炳闻,刘海萍,徐鹏,等.土壤标准样品中有机氯农药的加速溶剂萃取-净化方法优化[J].中国测试,2015,41(3):55-60.
[9]国家质量监督检验检疫总局.标准样品工作导则(3)标准样品定值的一般原则和统计方法:GB/T 15000.3—2008[S].北京:中国标准出版社,2008.
[10]李宁,郭健,王倩,等.趋势分析法评价苯系物标准气体的时间稳定性[J].中国环境监测,2012,28(5):130-133.
[2]国家质量监督检验检疫总局.地表水环境质量标准:GB 3838—2002[S].北京:中国环境科学出版社,2002.
[3]黄林艳,刘海萍,赵亚娴,等.环境基质有机标准样品研究进展[J].环境化学,2017,36(10):2 115-2 125.
[4]赵云芝,谢振伟,潘乐丹,等.固相萃取/液相色谱-串联质谱法测定水中苯胺类化合物及基质干扰的消除[J].色谱,2016,34(2):289-298.
[5]周琛,骆春迎,余辉菊,等.直接进样-液相色谱-串联质谱法同时测定水中的5种苯胺类化合物[J].分析化学,2016,44(6):935-941.
[6]朱颖,刘沛,秦迪岚,等.液液萃取-高效液相色谱法测定水中苯胺和联苯胺[J].理化检验-化学分册,2016,52(7):840-842.
[7]生态环境部.水质苯胺类化合物的测定液液萃取/液相色谱法(征求意见稿)[S].http://www.doc88.com/p-2901793008632.html.
[8]鲁炳闻,刘海萍,徐鹏,等.土壤标准样品中有机氯农药的加速溶剂萃取-净化方法优化[J].中国测试,2015,41(3):55-60.
[9]国家质量监督检验检疫总局.标准样品工作导则(3)标准样品定值的一般原则和统计方法:GB/T 15000.3—2008[S].北京:中国标准出版社,2008.
[10]李宁,郭健,王倩,等.趋势分析法评价苯系物标准气体的时间稳定性[J].中国环境监测,2012,28(5):130-133.