Purity Determination of Triclosan by Proton-Nuclear Magnetic Resonance
摘 要
以丙烯酰胺为内标,氘代二甲基亚砜(DMSO-d6)为溶剂,对用1H核磁共振法测定三氯生纯度条件进行试验。在脉冲延迟时间20 s和扫描次数64等条件下得到1H-NMR谱图。选择H-11(δ 6.88)和δ 5.59分别作为样品和内标的定量峰,取其积分峰面积平均值按公式计算三氯生的纯度。结果表明:样品与内标物的质量比在1.01~10.16内,与其定量峰面积比值呈线性关系。平行测定同一样品6份,按所得样品对内标物定量峰面积的比值,计算其相对标准偏差(n=6)为0.12%。按所提出方法分析了三氯生实样,结果的平均值(n=3)为99.78%,与质量平衡法所得结果(99.81%)相符。
Abstract
A study on the application of 1H-NMR spectroscopy to the determination of purity of triclosan (TCS), by using acrylamide as internal standard and DMSO-d6 as solvent, was made, and the 1H-NMR spectrum was obtained under the conditions of time of pulse delay of 20 s and scanning time of 64. H-11 (δ 6.88) and δ 5.59 were selected as the quantitative peaks for the sample and the internal standard. Averages of integrals of the peak areas were taken and used for calculation of purity of TCS by the formula given. As shown by the result, linear relationship was obtained between values of mass ratios of sample (mr) to internal standard (ms) ranged between 1.01 and 10.16 and respective values of ratios of integrals of peak areas of sample (Ar) to internal standard (As). Six portions of a same TCS sample were taken and analyzed by 1H-NMR in parallel, values of ratios of peak areas of samples to internal standard were taken, and value of RSD (n=6) found was 0.12%. A TCS sample was analyzed by the proposed method for its purity, and average value of the results (n=3) found was 99.78%, which was in consistency with the results found by mass balance method (99.81%).
中图分类号 O657.2 DOI 10.11973/lhjy-hx201807006
所属栏目 工作简报
基金项目 上海市技术性贸易措施应对专项(15TBT009)
收稿日期 2017/7/10
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备注李永利,高级工程师,主要从事有机分析研究工作,jinchi333@126.com
引用该论文: LI Yongli,WU Jianjun,LI Jie,XU Zhuoni,CHEN Ying. Purity Determination of Triclosan by Proton-Nuclear Magnetic Resonance[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(7): 770~773
李永利,吴建军,李杰,许卓妮,陈鹰. 1H核磁共振法测定三氯生的纯度[J]. 理化检验-化学分册, 2018, 54(7): 770~773
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参考文献
【1】郑欣,刘婷婷,王一喆,等.三氯生毒性效应及水质基准研究进展[J].生态环境学报, 2016,25(3):539-546.
【2】周艳君,施阳,吴源.三氯生和三氯卡班的毒性研究进展[J].安徽医科大学学报, 2017,52(1):147-151.
【3】黄珍茹,王彩凤,田英.三氯生在环境与人体中的暴露情况研究进展[J].环境与职业医学, 2015,32(8):795-800.
【4】CHRISTEN V, CRETTAZ P, OBERLI-SCHRÄMMLI A, et al. Some flame retardants and the antimicrobials triclosan and triclocarban enhance the androgenic activity in vitro[J]. Chemosphere, 2010,81(10):1245-1252.
【5】XIA K, HUNDAL L S, KUMAR K, et al. Tricarban, triclosan, polybrominated diphenyl ethers, and 4-nonylphenol in biosolids and in soil receiving 33-year biosolids application[J]. Environmental Toxicology & Chemistry, 2010,29(3):597-605.
【6】解娜,丁晓静,宋宝花,等.胶束电动毛细管色谱法同时测定复方化学消毒剂及日化产品中邻苯二甲醛、对氯间二甲基苯酚及三氯生[J].色谱, 2013,31(1):64-70.
【7】符策奕,梁颖,许文佳,等.液相色谱串联质谱法同时测定6类不同剂型化妆品中10种防腐剂[J].药物分析杂志, 2016,36(8):1456-1464.
【8】李丕,郭项雨,李海玉,等.高效液相色谱法测定洗涤用品中三氯生和三氯卡班[J].分析试验室, 2014,33(12):1416-1419.
【9】刘湘军,赵妍,赵珊,等.超高效液相色谱-串联质谱法同时测定日化产品中的三氯生与三氯卡班[J].分析测试学报, 2013,32(1):64-68.
【10】张品,张晶,石莹,等.固相萃取-超高效液相色谱-串联质谱法测定母乳中三氯生和三氯卡班[J].卫生研究, 2015,44(2):294-298.
【11】周雪飞,陈家斌,周世兵,等.污水处理系统中三氯生固相萃取(SPE)-气相色谱(GC)-电子俘获检测器(ECD)测定方法的建立和优化[J].环境化学, 2011,30(2):506-510.
【12】韩超,黄芙珍,李舟,等.基于固相萃取-液相色谱-串联质谱法的纺织品中三氯生和三氯卡班的测定[J].纺织学报, 2014,35(4):71-74.
【13】吴先富,张琪,马玲云,等.定量核磁共振法测定去水卫矛醇的含量[J].药物分析杂志, 2017,37(1):181-184.
【14】张奉民,丁克鸿,陶文波.定量核磁共振技术测定嘧菌酯的含量[J].分析试验室, 2017,36(2):150-153.
【2】周艳君,施阳,吴源.三氯生和三氯卡班的毒性研究进展[J].安徽医科大学学报, 2017,52(1):147-151.
【3】黄珍茹,王彩凤,田英.三氯生在环境与人体中的暴露情况研究进展[J].环境与职业医学, 2015,32(8):795-800.
【4】CHRISTEN V, CRETTAZ P, OBERLI-SCHRÄMMLI A, et al. Some flame retardants and the antimicrobials triclosan and triclocarban enhance the androgenic activity in vitro[J]. Chemosphere, 2010,81(10):1245-1252.
【5】XIA K, HUNDAL L S, KUMAR K, et al. Tricarban, triclosan, polybrominated diphenyl ethers, and 4-nonylphenol in biosolids and in soil receiving 33-year biosolids application[J]. Environmental Toxicology & Chemistry, 2010,29(3):597-605.
【6】解娜,丁晓静,宋宝花,等.胶束电动毛细管色谱法同时测定复方化学消毒剂及日化产品中邻苯二甲醛、对氯间二甲基苯酚及三氯生[J].色谱, 2013,31(1):64-70.
【7】符策奕,梁颖,许文佳,等.液相色谱串联质谱法同时测定6类不同剂型化妆品中10种防腐剂[J].药物分析杂志, 2016,36(8):1456-1464.
【8】李丕,郭项雨,李海玉,等.高效液相色谱法测定洗涤用品中三氯生和三氯卡班[J].分析试验室, 2014,33(12):1416-1419.
【9】刘湘军,赵妍,赵珊,等.超高效液相色谱-串联质谱法同时测定日化产品中的三氯生与三氯卡班[J].分析测试学报, 2013,32(1):64-68.
【10】张品,张晶,石莹,等.固相萃取-超高效液相色谱-串联质谱法测定母乳中三氯生和三氯卡班[J].卫生研究, 2015,44(2):294-298.
【11】周雪飞,陈家斌,周世兵,等.污水处理系统中三氯生固相萃取(SPE)-气相色谱(GC)-电子俘获检测器(ECD)测定方法的建立和优化[J].环境化学, 2011,30(2):506-510.
【12】韩超,黄芙珍,李舟,等.基于固相萃取-液相色谱-串联质谱法的纺织品中三氯生和三氯卡班的测定[J].纺织学报, 2014,35(4):71-74.
【13】吴先富,张琪,马玲云,等.定量核磁共振法测定去水卫矛醇的含量[J].药物分析杂志, 2017,37(1):181-184.
【14】张奉民,丁克鸿,陶文波.定量核磁共振技术测定嘧菌酯的含量[J].分析试验室, 2017,36(2):150-153.
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