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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 more accurate and practical pretreatment method for the determination of fluoride in bone samples. Methods Using the new pretreatment device developed by the project, the bone samples that had been dried at 110 ℃ for 4 h were acid-distilled and the Latin square design was used. The recovery rate was used as an index to select the experimental conditions. The pretreatment method The experimental conditions of the factors (such as the amount of sulfuric acid added, the eluent and the alkalinity of the receiving solution) were investigated. The accuracy and precision of the bone samples from the rats exposed to fluoride were determined by using the best experimental conditions. Results When the amount of sulfuric acid was 200μl and the alkalinity of both eluent and receiving solution were both 1.2 mol / L, the average recovery was the highest (96.67 ± 6.04)%, which was the best one Experimental conditions. The accuracy and precision of the bone samples were tested using the above optimal experimental conditions. The relative standard deviations (RSDs) of the methods were within 5.5% and the recovery rates were 94% -102%. Conclusion Dry distillation - fluorine electrode method has good accuracy and precision, and compared with other traditional methods, the experimental device is simple and compact, less sample and reagent use, and can achieve large quantities of experimental determination, has a good practical Application prospects.