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| Determination of Metal Elements in Solid Chinese Veterinary Medicine Preparations by Inductively Coupled Plasma Emission Spectrometry (ICP-OES) with Microwave Digestion |
| Received:May 30, 2023 Revised:December 28, 2023 |
| View Full Text View/Add Comment Download reader |
| DOI：10.3969/j.issn.2095-1035.2024.04.017 |
| KeyWord:Microwave digestion; Solid preparations; Chinese veterinary medicine; Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES) |
| Author | Institution |
| LIU Zhan-tong |
河南省农畜水产品检验技术研究院 |
| ZHANG Chong-wei |
河南省农畜水产品检验技术研究院 |
| HAN Li |
河南省农畜水产品检验技术研究院 |
| LI Na |
河南省农畜水产品检验技术研究院 |
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| Abstract: |
| In order to achieve accurate determination of metal elements in solid Chinese veterinary drug preparations, nitric acid-hydrogen peroxide and microwave digestion were used for pretreating the samples. After digestion, the digestion tube was placed in the acid-driven processor at 170 degree Celsius to remove the acid. Combining microwave digestion and inductively coupled plasma optical emission spectrometry (ICP-OES) for the determination of the 14 elements, namely chromium, arsenic, cadmium, lead, sodium, magnesium, potassium, manganese, iron, copper, zinc, selenium, calcium, 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 is 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 are between 0.001-0.01 μg/mL, the concentration of manganese, copper and selenium are between 0.002-0.02 μg/mL, the concentration of iron and zinc are between 0.1-1.0 μg/mL, the concentration of magnesium and calcium are between 1.0-10.0 μg/mL, and the concentration of sodium, potassium and phosphorus are between 2.0-50.0 μg/mL, there is a good linear relationship, and the correlation coefficient (r) is greater than 0.9990. The detection limit of each element method is between 0.1-1.0 mg/kg, and the average recovery rate is in 90.0%～110.0%, the precision RSD is less than 10% (n=5). The method has the advantages of simple and quick pretreatment, low interference, good reproducibility, high sensitivity, and can test multiple elements simultaneously, and it can meet the demand for batch determination of the 14 elements(chromium, arsenic, cadmium, lead, sodium, magnesium, potassium, manganese, iron, copper, zinc, selenium, calcium, phosphorus) in solid Chinese veterinary drug preparations. |
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