砷铈催化光度法测定血清碘的样品消化方法

Sample preparation for iodine measurement by arsenic cerium catalytic spectrophotometry

目的：为研制血清中碘的砷铈催化光度测定标准方法筛选血清碘样品消化方法，并对新制定的血清中碘的砷铈催化光度测定方法进行方法学检验。方法方法学评价。以几种常用的样品消化剂进行血清碘的样品消化方法实验研究。血清样品经过消化处理后，以砷铈催化光度法测定碘浓度。对新制定砷铈催化光度法的线性范围、检测限、精密度、回收率及抗干扰能力进行检验。结果经筛选列入血清碘测定的新制定砷铈催化光度法的样品前处理方式为：以高氯酸－氯酸钠溶液为消化剂在130℃下消化120 min。新制定方法砷铈反应在13～30℃范围内选择任一稳定的温度及固定的反应时间都有碘质量浓度（ C）与测定A值对数值的定量线性关系C＝a＋blgA，线性范围为0～300μg／L（r＝－0．9996～－0．9999），检测限为2．2μg／L。测定3份血清的批内变异系数分别为0．70％、0．70％、0．74％（n＝6），批间变异系数分别为0．57％、0．51％、0．57％（n＝6），加标回收率范围为92．3％～105．8％，总平均回收率为97．9％。结论血清碘测定的新制定砷铈催化光度法具有良好的精密度和准确度，其样品消化剂容易配制易于贮备，使用仪器简单易操作，方法可成为易推广的血清碘检测可靠技术方法。（中华检验医学杂志，2017，40：119－125）

Objective To screen the suitable sample digestion method for measuring iodine in serum by arsenic cerium catalytic spectrophotometric method , and to carry out the methodology test for the newly developed arsenic cerium catalytic spectrophotometry for determination of iodine in serum .Methods Methodology evaluation.Experimentswere on the sample on the sample digestion method of serum iodine with several common digestive agents . After digestion treatment , the concentration of iodine in serum was determined by arsenic cerium catalytic spectrophotometry .The linearity and linear range of the standard curve, detection limit, precision, recovery rate and anti -interference ability of the newlydeveloped arsenic cerium catalytic spectrophotometry were tested .Results Sample pretreatment method included in the newly developed arsenic cerium catalytic spectrophotometry was selected as follows： perchloric acid -sodium chlorate solution was used as the digestive agent to digest 120 min at 130℃.The calibration relation of C =a＋blgA（ C： iodine concentration ,A： measuring absorbance ） of the newly developed method existed when arsenic ceriumcatalytic reaction was kept at a certain stable temperature range from 13℃ to 30℃ and in certain stable reacting time .The linear range of the calibration curvewas 0 -300 μg/Land the linear correlative coefficient was -0.9996 --0.9999.The intra assay coefficients of variation （ CVs ） were 0.70%,0.70%and 0.74%（n=6）, and the inter assay CVs were 0.57%, 0.51% and 0.57% （n=6） for 3 serum samples.The average recovery was 97.9% with a range from 92.3% to 105.8% for 3 serum samples.Conclusions The newly developed arsenic cerium catalytic spectrophotometry has good precision and accuracy .The sample digestion agent is easy to be prepared and reserved , and the instrument is simple and easy to be operated .The method can be widely used as a reliable technique for measuring iodine in serum.