高效液相色谱法测定合成橡胶材料中两种胍类硫化促进剂残留量的研究
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摘要
建立了一种快速测定合成橡胶材料中1,3-二苯胍(DPG)和1,3-二邻甲苯胍(DOTG)2种胍类硫化促进剂残留量的高效液相色谱法(HPLC)。样品以甲醇作溶剂经索氏抽提后,以C18色谱柱分离,乙腈和磷酸缓冲盐为流动相进行梯度洗脱,紫外检测波长为235 nm,外标法定量。该方法中DPG和DOTG在2~50 mg/L质量浓度范围内呈良好的线性关系,相关系数均为0.999 9,方法检出限分别为30 mg/kg和40 mg/kg。在10、20、40 mg/L加标水平下,样品的平均加标回收率为82.4%~94.5%,相对标准偏差(RSD,n=5)为1.0%~3.3%。该方法简单、快速、可靠性高,适用于合成橡胶材料中DPG和DOTG残留量的测定。
A new method was established for the determination of two kinds of guanidines vulcanization accelerators,1,3-diphenyl guanidine(DPG) and 1,3-di-o-tolylguanidine(DOTG) in synthetic rubber materials by high performance liquid chromatography(HPLC). The samples were extracted by soxhlet extraction with methanol,and separated on a C18 column with acetonitrile-phosphate buffer as mobile phase by gradient elution. The UV detection wavelength was set at 235 nm,and the external standard method was used for quantitative analysis. There were good linear relationships for the two componds in the concentration range of 2-50 mg/L with their correlation coefficients both 0. 999 9.The limits of detection of the method(MLODs) were 30 mg/kg and 40 mg/kg,respectively. The average recoveries for the analytes were in the range of 82. 4%-94. 5%,with the relative standard deviations(RSD,n = 5) of 1. 0%-3. 3%. This method was simple,rapid and reliable,and was suitable for the determination of DPG and DOTG residues in synthetic rubber materials.
A new method was established for the determination of two kinds of guanidines vulcanization accelerators,1,3-diphenyl guanidine(DPG) and 1,3-di-o-tolylguanidine(DOTG) in synthetic rubber materials by high performance liquid chromatography(HPLC). The samples were extracted by soxhlet extraction with methanol,and separated on a C18 column with acetonitrile-phosphate buffer as mobile phase by gradient elution. The UV detection wavelength was set at 235 nm,and the external standard method was used for quantitative analysis. There were good linear relationships for the two componds in the concentration range of 2-50 mg/L with their correlation coefficients both 0. 999 9.The limits of detection of the method(MLODs) were 30 mg/kg and 40 mg/kg,respectively. The average recoveries for the analytes were in the range of 82. 4%-94. 5%,with the relative standard deviations(RSD,n = 5) of 1. 0%-3. 3%. This method was simple,rapid and reliable,and was suitable for the determination of DPG and DOTG residues in synthetic rubber materials.
引文
[1]Wei F X,Zhang W G,Fan J,Yin X.Chem.World(韦凤仙,章伟光,范军,殷霞.化学世界),2007,8:504.
[2]Xu Q H,Xue X J.Chin.Rubber(徐清华,薛香菊.中国橡胶),2017,33(7):44-45.
[3]Yuan X H,Le J Y,Shen Y Z,Sun J L,Yang Y H.J.Toxicol.(袁学洪,乐俊仪,沈芸芝,孙建林,杨逸鸿.卫生毒理学杂志),1994,8(2):99-100.
[4]Wang W H,Xiang H L,Li L F.Chin.J.Dermatovenereol(王文慧,向海炼,李邻峰.中国皮肤性病学杂志),2016,30(10):1003-1006.
[5]Qu J B,Yang Y X,Chen C,Wang B W,Zheng Y D,Ren J.Chin.Synth.Rubber Ind.(曲静波,杨延翔,陈超,王葆葳,郑轶丹,任静.合成橡胶工业),2013,6:420-423.
[6]Xie Z L.Chin.Rubber Ind.(谢忠麟.橡胶工业),2016,63(9):567-573.
[7]Xie Z L.Chin.Rubber Ind.(谢忠麟.橡胶工业),2016,63(10):627-633.
[8]Xie Z L.Chin.Rubber Ind.(谢忠麟.橡胶工业),2016,63(11):699-702.
[9]Li L F,Bai Y N,Lei M,Liu L.Prog.Chem.(李龙飞,摆音娜,雷鸣,刘力.化学进展),2015,27(10):1500-1508.
[10]Rong J F,Mao S L,Zhong J H,Li J F,Huang Q L,Zou Q,Zhang Y J,Chen X C.J.Instrum.Anal.(荣杰峰,毛树禄,钟坚海,李军法,黄秋兰,邹强,张云金,陈学灿.分析测试学报),2016,35(4):438-442.
[11]Rong J F,Mao S L,Li J F,Zhong J H,Huang Q L,Zou Q,Zhang Y J,Chen X C.Phys.Test.Chem.Anal.:Chem.Anal.(荣杰峰,毛树禄,李军法,钟坚海,黄秋兰,邹强,张云金,陈学灿.理化检验-化学分册),2016,52(7):750-755.
[12]Tong Y G,Fang G W,Huang P.Chin.Rubber Ind.(童玉贵,方光伟,黄萍.橡胶工业),2013,60:754-756.
[13]Snyder L R,Kirkland J J,Dolan J W.Introduction to Modern Liquid Chromatography.3rd ed.Chen X M,Tang Y Y,transl.Beijing:People’s Health Press(劳埃德R.斯奈德,约瑟夫·柯克兰,约翰·W·多兰.现代液相色谱技术导论.3版.陈小明,唐雅妍,译.北京:人民卫生出版社),2012.
[14]Xia Y Y.Practical Manual for Inspector.3rd ed.Beijing:Chemical Industry Press(夏玉宇.化验员实用手册.3版.北京:化学工业出版社),2012.
[15]Liu Z.Instrumental Analysis.4th ed.Beijing:Chemical Industry Press(刘珍.仪器分析.4版.北京:化学工业出版社),2007.
[16]Zou H F,Zhang Y K,Lu P Z.High Performance Liquid Chromatography.Beijing:Science Press(邹汉法,张玉奎,卢佩章.高效液相色谱法.北京:科学出版社),1998:38.
[17]Chen L W,Wu C S,Wang Y,Wu Y L,Wang L,Dong H,Wang B,Luo H Y.J.Instrum.Anal.(陈立伟,吴楚森,汪毅,吴玉銮,王莉,董浩,王斌,罗海英.分析测试学报),2016,35(2):206-212.
[18]HG/T 2342-2010.Vulcanizing Accelerator DPG.Chemical Industry Standard of the People’s Republic of China(硫化促进剂DPG.中华人民共和国化工行业标准).
[19]Wei C M.Study on the Synthesis and Crystal Structure of Guanidine Derivatives.Nanjing:Nanjing Tech University(韦长梅.胍基化合物的合成与晶体结构研究.南京:南京工业大学),2004.
[2]Xu Q H,Xue X J.Chin.Rubber(徐清华,薛香菊.中国橡胶),2017,33(7):44-45.
[3]Yuan X H,Le J Y,Shen Y Z,Sun J L,Yang Y H.J.Toxicol.(袁学洪,乐俊仪,沈芸芝,孙建林,杨逸鸿.卫生毒理学杂志),1994,8(2):99-100.
[4]Wang W H,Xiang H L,Li L F.Chin.J.Dermatovenereol(王文慧,向海炼,李邻峰.中国皮肤性病学杂志),2016,30(10):1003-1006.
[5]Qu J B,Yang Y X,Chen C,Wang B W,Zheng Y D,Ren J.Chin.Synth.Rubber Ind.(曲静波,杨延翔,陈超,王葆葳,郑轶丹,任静.合成橡胶工业),2013,6:420-423.
[6]Xie Z L.Chin.Rubber Ind.(谢忠麟.橡胶工业),2016,63(9):567-573.
[7]Xie Z L.Chin.Rubber Ind.(谢忠麟.橡胶工业),2016,63(10):627-633.
[8]Xie Z L.Chin.Rubber Ind.(谢忠麟.橡胶工业),2016,63(11):699-702.
[9]Li L F,Bai Y N,Lei M,Liu L.Prog.Chem.(李龙飞,摆音娜,雷鸣,刘力.化学进展),2015,27(10):1500-1508.
[10]Rong J F,Mao S L,Zhong J H,Li J F,Huang Q L,Zou Q,Zhang Y J,Chen X C.J.Instrum.Anal.(荣杰峰,毛树禄,钟坚海,李军法,黄秋兰,邹强,张云金,陈学灿.分析测试学报),2016,35(4):438-442.
[11]Rong J F,Mao S L,Li J F,Zhong J H,Huang Q L,Zou Q,Zhang Y J,Chen X C.Phys.Test.Chem.Anal.:Chem.Anal.(荣杰峰,毛树禄,李军法,钟坚海,黄秋兰,邹强,张云金,陈学灿.理化检验-化学分册),2016,52(7):750-755.
[12]Tong Y G,Fang G W,Huang P.Chin.Rubber Ind.(童玉贵,方光伟,黄萍.橡胶工业),2013,60:754-756.
[13]Snyder L R,Kirkland J J,Dolan J W.Introduction to Modern Liquid Chromatography.3rd ed.Chen X M,Tang Y Y,transl.Beijing:People’s Health Press(劳埃德R.斯奈德,约瑟夫·柯克兰,约翰·W·多兰.现代液相色谱技术导论.3版.陈小明,唐雅妍,译.北京:人民卫生出版社),2012.
[14]Xia Y Y.Practical Manual for Inspector.3rd ed.Beijing:Chemical Industry Press(夏玉宇.化验员实用手册.3版.北京:化学工业出版社),2012.
[15]Liu Z.Instrumental Analysis.4th ed.Beijing:Chemical Industry Press(刘珍.仪器分析.4版.北京:化学工业出版社),2007.
[16]Zou H F,Zhang Y K,Lu P Z.High Performance Liquid Chromatography.Beijing:Science Press(邹汉法,张玉奎,卢佩章.高效液相色谱法.北京:科学出版社),1998:38.
[17]Chen L W,Wu C S,Wang Y,Wu Y L,Wang L,Dong H,Wang B,Luo H Y.J.Instrum.Anal.(陈立伟,吴楚森,汪毅,吴玉銮,王莉,董浩,王斌,罗海英.分析测试学报),2016,35(2):206-212.
[18]HG/T 2342-2010.Vulcanizing Accelerator DPG.Chemical Industry Standard of the People’s Republic of China(硫化促进剂DPG.中华人民共和国化工行业标准).
[19]Wei C M.Study on the Synthesis and Crystal Structure of Guanidine Derivatives.Nanjing:Nanjing Tech University(韦长梅.胍基化合物的合成与晶体结构研究.南京:南京工业大学),2004.