三氯卡班纯度标准物质的定值及不确定度分析
|
摘要
建立了三氯卡班纯度标准物质的定值分析、不确定度评定和制备方法。采用两种不同原理的测试方法(质量平衡法和定量核磁共振法)对三氯卡班进行了纯度定值研究,运用液相色谱法对三氯卡班的分装样品进行均匀性检验和稳定性考察(包括短期运输条件稳定性和长期储存条件稳定性),并评定了不确定度。统计结果表明三氯卡班纯度标准物质在95%的置信区间具有良好的均匀性和稳定性。三氯卡班纯度标准物质定值结果的标准值和相对扩展不确定度分别为99. 3%和0. 5%(k=2),对于检验检测工作中三氯卡班的准确测量具有重要意义。
The method for value determination,uncertainty evaluation and preparation of purity reference material of triclocarban was established.The quantitative analysis was carried out by means of quantitative nuclear magnetic resonance( q NMR) and mass balance method simultaneously.The homogeneity examination and stability investigation( including short-term transport condition and long-term storage condition) of the triclocarbans sample was conducted with liquid chromatography method.The purity reference material of trichlorocarban had good uniformity and stability in the 95% confidence interval.The certified value of the purity reference material of triclocarban was 99. 3% with an relative expanded uncertainty of 0. 5%( k = 2),which would assure the accuracy of determination of triclocarban.
The method for value determination,uncertainty evaluation and preparation of purity reference material of triclocarban was established.The quantitative analysis was carried out by means of quantitative nuclear magnetic resonance( q NMR) and mass balance method simultaneously.The homogeneity examination and stability investigation( including short-term transport condition and long-term storage condition) of the triclocarbans sample was conducted with liquid chromatography method.The purity reference material of trichlorocarban had good uniformity and stability in the 95% confidence interval.The certified value of the purity reference material of triclocarban was 99. 3% with an relative expanded uncertainty of 0. 5%( k = 2),which would assure the accuracy of determination of triclocarban.
引文
[1]纪春,张丽珍,牛伟,等.三氯卡班研究现状与展望[J].山西农业科学,2010,38(10):82-87.
[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]金欢孝,邵波,许惠英,等.三氯卡班胁迫对淡水藻生理生化的影响[J].浙江树人大学学报(自然科学版),2016,16(4):21-25.
[4]SCHEBB N H,MUVVALA J B,MORIN D,et al.Metabolic activation of the antibacterial agent triclocarban by cytochrome P450 1A1 yielding glutathione adducts[J].Drug Metab.Dispos.,2014,42(7):1 098-1 102.
[5]XIA K,HUNDAL L S,KUMAR K,et al.Triclocarban,triclosan,polybrominated diphenyl ethers,and 4-nonylphenol in biosolids and in soil receiving 33-year biosolids application[J]. Environ. Toxicol. Chem.,2010,29(3):597-605.
[6]马康,杨冉,王海峰.质量平衡法分析1,2,3,4-四氯苯的纯度分析与不确定度评定[J].岩矿测试,2013,32(2):334-339.
[7]马康,苏福海,王海峰.有机纯度标准物质定值技术研究进展[J].分析测试学报,2013,32(7):901-908.
[8]宋印清,王敏,周剑.甲硝唑标准物质的纯度定值分析与不确定度评估研究[J].化学试剂,2016,38(11):1 095-1 098.
[9]黄挺,张伟,全灿,等.定量核磁共振法研究进展[J].化学试剂,2012,34(4):327-341.
[10]国家标准物质研究中心.一级标准物质研制技术规范:JJF1006—1994[S].北京:中国计量出版社,1994.
[11]全国质量监督检验检疫总局.标准物质定值的通用原则及统计学原理:JJF 1343—2012[S].北京:中国质检出版社,2012.
[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]金欢孝,邵波,许惠英,等.三氯卡班胁迫对淡水藻生理生化的影响[J].浙江树人大学学报(自然科学版),2016,16(4):21-25.
[4]SCHEBB N H,MUVVALA J B,MORIN D,et al.Metabolic activation of the antibacterial agent triclocarban by cytochrome P450 1A1 yielding glutathione adducts[J].Drug Metab.Dispos.,2014,42(7):1 098-1 102.
[5]XIA K,HUNDAL L S,KUMAR K,et al.Triclocarban,triclosan,polybrominated diphenyl ethers,and 4-nonylphenol in biosolids and in soil receiving 33-year biosolids application[J]. Environ. Toxicol. Chem.,2010,29(3):597-605.
[6]马康,杨冉,王海峰.质量平衡法分析1,2,3,4-四氯苯的纯度分析与不确定度评定[J].岩矿测试,2013,32(2):334-339.
[7]马康,苏福海,王海峰.有机纯度标准物质定值技术研究进展[J].分析测试学报,2013,32(7):901-908.
[8]宋印清,王敏,周剑.甲硝唑标准物质的纯度定值分析与不确定度评估研究[J].化学试剂,2016,38(11):1 095-1 098.
[9]黄挺,张伟,全灿,等.定量核磁共振法研究进展[J].化学试剂,2012,34(4):327-341.
[10]国家标准物质研究中心.一级标准物质研制技术规范:JJF1006—1994[S].北京:中国计量出版社,1994.
[11]全国质量监督检验检疫总局.标准物质定值的通用原则及统计学原理:JJF 1343—2012[S].北京:中国质检出版社,2012.