微波消解-电感耦合等离子体发射光谱(ICP-OES)法测定固体中兽药制剂中金属元素

Determination of Metal Elements in Solid Chinese Veterinary Medicine Preparations by Inductively Coupled Plasma Optical Emission Spectrometry(ICP-OES)with Microwave Digestion

传统的中兽药制剂中金属元素检测主要为原子吸收光谱法或原子荧光光谱法等单一元素检测方法,为提高检测效率,实现对固体中兽药制剂中金属元素的准确测定,使用硝酸-过氧化氢及微波消解进行样品前处理,消解后置消解管于赶酸仪中170℃赶酸,采用微波消解-电感耦合等离子体发射光谱(ICP-OES)法相结合对固体兽药制剂中铬、砷、镉、铅、钠、镁、钾、锰、铁、铜、锌、硒、钙、磷等14种元素同时测定,轴向观测方向,内标法定量。消解及赶酸效果理想,整个过程安全、高效、无损。对消解方式进行了考察,并对消解酸体系及消解温度进行了优化,选择了最优的赶酸温度及元素分析谱线,同时也通过试剂加标回收、样品加标回收、样品处理液加标回收相比较的方式验证了方法的可行性。结果表明,铅、镉、铬、砷在0.001~0.01μg/mL,锰、铜、硒在0.002~0.02μg/mL,铁、锌在0.1~1.0μg/mL,镁、钙在1.0~10.0μg/mL,钠、钾、磷在2.0~50.0μg/mL线性关系良好,相关系数(r)均大于0.999,各元素方法检出限在0.1~1.0 mg/kg,平均回收率在90.0%~110%,精密度RSD小于10%(n=5)。方法前处理简便快捷、干扰小、重现性好、灵敏度高,可同时测定多种元素,满足批量测定固体中兽药制剂中铬、砷、镉、铅、钠、镁、钾、锰、铁、铜、锌、硒、钙、磷等14种元素定量分析的要求。

The traditional detection of metal elements in solid Chinese veterinary drug preparations mainly involves single element detection methods such as atomic absorption spectroscopy and atomic fluorescence spectroscopy.In order to improve detection efficiency and achieve accurate determination of metal elements in solid Chinese veterinary drug preparations,nitric acid-hydrogen peroxide and microwave digestion were used for pretreating the sample pretreatment.After digestion,the digestion tube was placed in the acid-driven processor at 170℃to remove the acid.Combining microwave digestion and inductively coupled plasma optical emission spectrometry(ICP-OES)for the determination of 14 elements(chromium,arsenic,cadmium,lead,sodium,magnesium,potassium,manganese,iron,copper,zinc,selenium,calcium and phosphorus)in solid Chinese veterinary drug preparations simultaneously,the direction of observation was horizontal,and internal standard method was adopted for quantification.The effects of digestion and acid removal were satisfactory,and the whole process was safe,efficient and non-destructive.The digestion method was reviewed,the digestion acid system and digestion temperature were optimized,and the optimal acid removal temperature and elemental analysis spectral line were selected.Meanwhile,the feasibility of the method was verified by comparison of reagent spiked recovery,sample spiked recovery,and sample treatment solution spiked recovery.The results showed that,when the concentration of lead,cadmium,chromium and arsenic were 0.001-0.01μg/mL,the concentration of manganese,copper and selenium were 0.002-0.02μg/mL,the concentration of iron and zinc were 0.1-1.0μg/mL,the concentration of magnesium and calcium were 1.0-10.0μg/mL,and the concentration of sodium,potassium and phosphorus were 2.0-50.0μg/mL.There was a good linear relationship,and the correlation coefficient(r)was greater than 0.9990.The detection limit of each element method was 0.1-1.0 mg/kg,the average recovery rate was 90.0%-110%,and the precision RSD was less than 10%(n=5).The method has the advantages of simple and quick pretreatment,low interference,good reproducibility,high sensitivity,and can determined simultaneously multiple elements,and it can meet the demand for batch determination of the above 14 elements in solid Chinese veterinary drug preparations.