Determination of Metal Elements in Solid Chinese Veterinary Medicine Preparations by Inductively Coupled Plasma Optical Emission Spectrometry(ICP-OES)with Microwave Digestion
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 0.001-0.01 μg/mL,the concentration of manganese,copper and selenium were 0.002-0.02 µg/mL,the concentration of iron and zinc were 0.1-1.0 μg/mL,the concentration of magnesium and calcium were 1.0-10.0 µg/mL,and the concentration of sodium,potassium and phosphorus were 2.0-50.0 μg/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.
万方数据
维普
