微量血清氟电极法测定过程中总离子强度调节缓冲液的对比与优化
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摘要
目的探讨4种总离子强度调节缓冲液(TISAB)对微量血清(大鼠血清和小牛血清)氟检测的影响,并进一步探索不同血清与TISAB的最佳混合比例。方法分别建立4种TISAB的标准曲线方程,分析TISAB种类对标准曲线的影响;将4种TISAB分别与加标血清样本(小牛血清和大鼠血清)1∶1体积混合后测定,分析TISAB种类对测定结果回收率的影响;最后改变血清与TISAB的体积比,根据回收率情况确定TISAB的最佳体积比。结果 TISABⅢ的标线拟合程度最好(R2=0.9926),且在大鼠血清的加标回收实验中的不同加标量回收率最好(90%~105%);TISABⅣ(卫生行业标准推荐)在小牛血清的加标回收实验中回收率最佳(90%~110%)。当大鼠血清样本与TISAB体积比改变时,每种TISAB均存在一个良好回收率的最佳比例,但其中只有TISABⅢ仍为1∶1时回收率最佳;而体积比改变对小牛血清的回收率改变效果不明显。结论卫生行业标准推荐方法只适合微量小牛血清类型样本的氟离子检测,而不适合微量大鼠血清氟化物的测定。
Objective To probe on the influence by four kinds of total ionic strength regulating buffer( TISAB) in establishing the standard curve and determining the level of fluoride in trace serum sample( rats serum and the calf serum) by fluoride ion selective electrode,and further explore the optimal volume ratio among TISAB and serum samples.Methods Standard curve equations of four TISAB were established to clarify the influence of TISAB kinds. And the trace serum samples( rats and calf) were diluted to 1times by TISAB,and then levels of fluoride in the samples that added by the standard sodium fluoride were detected,subsequently the influence of TISAB kinds on recovery rate were analyzed. Finally, the optimal ratio among serum sample and each TISAB in different serum was determined according to the recovery rate of the serum sample with different volume ratio. Results The standard curve of TISAB Ⅲ sample exhibited best fitting effect( R2= 0. 9926),and it also showed the overwhelming superiority with thescope of recovery rates ranged from 90 % to 105 % in the rat serum standard addition recovery experiments. As calf serum, TISAB Ⅳ( recommended by health industry standard) performed superior than others with the scope of recovery rate ranged from 90%to 110% in standard addition recovery experiment. When the volume ratio changed,every kinds of TISAB had an optimal proportion with good recovery rate,only TISAB Ⅲ with the proportion as 1 ∶ 1,nevertheless,those change little affected on the recovery rate in calf serum. Conclusion The method recommended by health industry standard is only suitable for detecting the trace amounts of fluoride in the serum sample as calf,but not the serum sample as rats.
Objective To probe on the influence by four kinds of total ionic strength regulating buffer( TISAB) in establishing the standard curve and determining the level of fluoride in trace serum sample( rats serum and the calf serum) by fluoride ion selective electrode,and further explore the optimal volume ratio among TISAB and serum samples.Methods Standard curve equations of four TISAB were established to clarify the influence of TISAB kinds. And the trace serum samples( rats and calf) were diluted to 1times by TISAB,and then levels of fluoride in the samples that added by the standard sodium fluoride were detected,subsequently the influence of TISAB kinds on recovery rate were analyzed. Finally, the optimal ratio among serum sample and each TISAB in different serum was determined according to the recovery rate of the serum sample with different volume ratio. Results The standard curve of TISAB Ⅲ sample exhibited best fitting effect( R2= 0. 9926),and it also showed the overwhelming superiority with thescope of recovery rates ranged from 90 % to 105 % in the rat serum standard addition recovery experiments. As calf serum, TISAB Ⅳ( recommended by health industry standard) performed superior than others with the scope of recovery rate ranged from 90%to 110% in standard addition recovery experiment. When the volume ratio changed,every kinds of TISAB had an optimal proportion with good recovery rate,only TISAB Ⅲ with the proportion as 1 ∶ 1,nevertheless,those change little affected on the recovery rate in calf serum. Conclusion The method recommended by health industry standard is only suitable for detecting the trace amounts of fluoride in the serum sample as calf,but not the serum sample as rats.
引文
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[2]刘璐,张颖,顾何峰,等.不同饮水氟浓度对大鼠生化指标影响[J].中国公共卫生,2014,30(11):1476-1478.
[3]吴晓蕾,张镖.毕节市燃煤污染区域8-12岁学生氟斑牙现状调查研究[J].慢性病学杂志,2015,16(3):325-328.
[4]李建国,李菊梅.氟离子选择电极法在测试中应注意的问题[J].分析试验室,2001,20(1):97-98.
[5]万红友,师会勤,周生路,等.总离子强度缓冲剂对含氟溶液测定的影响[J].土壤通报,2004,35(3):380-382.
[6]郜红建,张显晨,蔡荟梅,等.水中氟化物测定过程中总离子强度调节缓冲液的对比与优化[J].环境化学,2010,29(4):754-759.
[7]LAURA I P,RODOLFO C P,ALFREDO R.Potentiometric measurement of ionic,acid-labile and covalently bound fluorine[J].J Fluorine Chem,2007,128:1425-1428.
[8]张志瑜,瞿城,钱聪,等.高温燃烧水解氟电极法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.
[9]何爱桃,黄仁建,谢元甫,等.不同程度氟斑牙儿童血清无机元素含量分析[J].中国地方病预防杂志,2008,23(2):111-113.
[10]涂俊,刘克俭,李明峰,等.职业性氟接触人群血氟、尿氟水平及相关因素研究[J].中国工业医学杂志,2010,23(3):163-166.
[11]王婵娟,单可人,刘艳洁,等.毕节市人群乙肝感染状况及血氟含量检测[J].中国公共卫生,2009,25(8):1001-1002.