骨氟化物水平的干燥蒸馏-氟电极测定法的实验条件研究
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摘要
目的建立一种较为准确、实用的骨样本氟测定预处理方法。方法应用课题研发的新型预处理装置对已110℃干燥4 h后粉碎的骨样本进行酸蒸馏处理,使用拉丁方设计,以回收率作为选择实验条件的指标,对骨样本氟测定的预处理方法进行条件因素(硫酸加入量、淋洗液及接收液碱度值)的实验研究;并应用探索出的最佳实验条件对氟暴露大鼠的骨样本进行准确度和精密度测定。结果当硫酸加入量为200μl、淋洗液与接收液碱度均为1.2 mol/L时,样本组测定的平均回收率最高,为(96.67±6.04)%,即选定该条件为最佳测定实验条件;应用上述最佳实验条件对骨样本进行准确度和精密度检测,方法检测的相对标准偏差(RSD)均在5.5%以内,回收率为94%~102%。结论干燥蒸馏-氟电极法具有较好的准确度和精密度,且与其他传统方法相比,实验装置简单小巧,样本及药剂使用量少,并可实现大批量的实验测定,具有良好的实际应用前景。
[Objective] To establish a simple and suitable pre-treatment method for determining the contents of fluoride in bone sample.[Methods]The samples were dried under 110 ℃ for 4 hours and distilled by the new device which developed by our research group before,and then the fluoride contents were determined in 3 parallel tests under different volume of H2SO4,different molarity of leacheate and receptor fluid,adopting Latin square design and rate of recovery as the indexes of the research. The bone samples of rats exposed to fluoride were detected under the optimal experimental conditions,to analyze the accuracy and precision.[Results]The average value of recovery was highest(96.67±6.04)% when the experiment condition was200 μl H2SO4,1.2mol/L Na OH solution of leacheate and receptor fluid,which was regarded as the optimal conditions for determining of fluoride content. The relative standard deviations(RSD)were less than 5.5 % and the range of recovery rate was from 94 % to 102 % when applying the above experiment conditions.[Conclusion]The method describes above is simple and suitable with well accuracy and precision. Compared to the traditional methods,it has a good application prospect for saving the usage amount of the sample and reagent,as well as the realization of the quantity parallel test.
[Objective] To establish a simple and suitable pre-treatment method for determining the contents of fluoride in bone sample.[Methods]The samples were dried under 110 ℃ for 4 hours and distilled by the new device which developed by our research group before,and then the fluoride contents were determined in 3 parallel tests under different volume of H2SO4,different molarity of leacheate and receptor fluid,adopting Latin square design and rate of recovery as the indexes of the research. The bone samples of rats exposed to fluoride were detected under the optimal experimental conditions,to analyze the accuracy and precision.[Results]The average value of recovery was highest(96.67±6.04)% when the experiment condition was200 μl H2SO4,1.2mol/L Na OH solution of leacheate and receptor fluid,which was regarded as the optimal conditions for determining of fluoride content. The relative standard deviations(RSD)were less than 5.5 % and the range of recovery rate was from 94 % to 102 % when applying the above experiment conditions.[Conclusion]The method describes above is simple and suitable with well accuracy and precision. Compared to the traditional methods,it has a good application prospect for saving the usage amount of the sample and reagent,as well as the realization of the quantity parallel test.
引文
[1]World Health Organization(WHO),Fluoride in Drinking-water[EB/OL],WHO Press,Switzerland,2006.http://www.who.int/water_sanitation_health/publications/fluoride_drinking_water_full.pdf?ua=1.
[2]LIU GJ,YE QF,CHEN W,et al.Study of the relationship between the lifestyle of residents residing in fluorosis endemic areas and adult skeletal fluorosis[J].Environ Toxicol Pharmacol,2015,40(1):326-332.
[3]吴延莉,曾贝贝,韦艳,等.慢性氟中毒大鼠骨组织中AC-c AMP-PKA信号转导通路的表达[J].环境卫生学杂志,2014,4(5):419-423.
[4]梁伟江,张树球,李友晶,等.海尔福对氟中毒小鼠排氟和保护骨胶原蛋白的实验研究[J].中国地方病防治杂志,2003,18(6):339-341.
[5]张志瑜,瞿城,钱聪,等.高温燃烧水解氟电极测定骨氟化物水平实验条件的研究[J].中国地方病学杂志,2006,25(4):450-453.
[6]赵贵元,董宝山,李巧贤.工业氟污染区山羊骨氟变化的研究[J].畜牧与饲料科学,2010,31(6-7):192-194.
[7]VENKATESWARLU P.Determination of fluoride in bone by aluminum monofluoride molecular absorption spectrometry[J].Anal Chimica Acta,1992,262(1):33-40.
[8]NOGUCHI Y,ZHANG L,MARUTA T,et al.Simultaneous determination of fluorine,chlorine and bromine in cement with ion chromatography after pyrolysis[J].Anal Chimica Acta,2009,640(1-2):106-109.
[9]DRESSLER VL,POZEBON D,éDER LM FLORES,et al.Potentiometric determination of fluoride in geological and biological samples following pyrohydrolytic de composition[J].Anal Chimica Acta,2002,466(1):117-123.
[10]LEITEA GAS,SAWANA RMM,TEóFILOA JM,et al.Exposure to lead exacerbates dental fluorosis[J].Arch Oral Biol,2011,56(7):695-702.
[11]SAWAN RMM,LEITE GAS,SARAIVA MCP,et al.Fluoride increases lead concentrations in whole blood and in calcified tissues from leadexposed rats[J].Toxicology,2010,271(1-2):21-26.
[12]陈南.淡水鱼中氟的测定[J].江西食品科技,2010,(3):26-27.
[13]中华人民共和国卫生部,中国国家标准化管理委员会.食品中氟的测定:GB/T 5009.18-2003[S].北京:中国标准出版社,2004.
[14]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.煤中氟的测定方法:GB/T 4633-2014[S].北京:中国标准出版社,2004.
[2]LIU GJ,YE QF,CHEN W,et al.Study of the relationship between the lifestyle of residents residing in fluorosis endemic areas and adult skeletal fluorosis[J].Environ Toxicol Pharmacol,2015,40(1):326-332.
[3]吴延莉,曾贝贝,韦艳,等.慢性氟中毒大鼠骨组织中AC-c AMP-PKA信号转导通路的表达[J].环境卫生学杂志,2014,4(5):419-423.
[4]梁伟江,张树球,李友晶,等.海尔福对氟中毒小鼠排氟和保护骨胶原蛋白的实验研究[J].中国地方病防治杂志,2003,18(6):339-341.
[5]张志瑜,瞿城,钱聪,等.高温燃烧水解氟电极测定骨氟化物水平实验条件的研究[J].中国地方病学杂志,2006,25(4):450-453.
[6]赵贵元,董宝山,李巧贤.工业氟污染区山羊骨氟变化的研究[J].畜牧与饲料科学,2010,31(6-7):192-194.
[7]VENKATESWARLU P.Determination of fluoride in bone by aluminum monofluoride molecular absorption spectrometry[J].Anal Chimica Acta,1992,262(1):33-40.
[8]NOGUCHI Y,ZHANG L,MARUTA T,et al.Simultaneous determination of fluorine,chlorine and bromine in cement with ion chromatography after pyrolysis[J].Anal Chimica Acta,2009,640(1-2):106-109.
[9]DRESSLER VL,POZEBON D,éDER LM FLORES,et al.Potentiometric determination of fluoride in geological and biological samples following pyrohydrolytic de composition[J].Anal Chimica Acta,2002,466(1):117-123.
[10]LEITEA GAS,SAWANA RMM,TEóFILOA JM,et al.Exposure to lead exacerbates dental fluorosis[J].Arch Oral Biol,2011,56(7):695-702.
[11]SAWAN RMM,LEITE GAS,SARAIVA MCP,et al.Fluoride increases lead concentrations in whole blood and in calcified tissues from leadexposed rats[J].Toxicology,2010,271(1-2):21-26.
[12]陈南.淡水鱼中氟的测定[J].江西食品科技,2010,(3):26-27.
[13]中华人民共和国卫生部,中国国家标准化管理委员会.食品中氟的测定:GB/T 5009.18-2003[S].北京:中国标准出版社,2004.
[14]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.煤中氟的测定方法:GB/T 4633-2014[S].北京:中国标准出版社,2004.