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| 干灰化-氢化物发生原子荧光光谱检测植物油中砷含量的方法改进 |
| Method improvement for determination of arsenic in vegetable oil by dry ashing-hydride generation atomic fluorescence spectrometry |
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| DOI： |
| 中文关键词: 植物油 砷 干灰化法 前处理 改进 |
| 英文关键词:vegetable oil arsenic dry ashing pretreatment improvement |
| 基金项目: |
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| 中文摘要: |
| 对GB 5009.11—2014《食品安全国家标准 食品中总砷及无机砷的测定》第二法中氢化物发生原子荧光光谱法的干灰化法前处理上的操作细节进行补充和明确，对实验参数进行优化，并对实际样品进行了测定。在确保数据准确性的基础上，研究了称样量、硝酸镁添加量及添加形式、加防爆沸珠、炭化过程、灰化温度和灰化时间对实验的影响。结果表明，优化后的前处理条件为：称样量4 g；添加10 mL、400 g/L的硝酸镁溶液；加入防爆沸珠；90~110 ℃将水分蒸干，180~250 ℃将样品炭化至干渣，加入氧化镁后300～350 ℃加热至样品底部为灰色或白色；灰化温度540 ℃；灰化时间8 h。改进后实验方法的加标回收率为100.0%~106.0%，相对标准偏差为1.88%～11.78%。改进后的实验方法能准确测定植物油中的痕量砷。 |
| 英文摘要: |
| The operation details of dry ashing pretreatment of hydride generation atomic fluorescence spectrometry in the second method of GB 5009.11—2014 Food safety of national standard determination of total arsenic and inorganic arsenic in food were supplemented and clarified. The experimental parameters were optimized and the actual samples were determined. On the basis of ensuring the accuracy of the data, the effects of sample mass, dosage and adding form of magnesium nitrate, adding anti-boiling beads, carbonization process, ashing temperature and ashing time on the experiment were studied. The results showed that the optimal pretreatment conditions were obtained as follows: sample mass 4 g, adding 10 mL 400 g/L magnesium nitrate solution, adding anti-boiling beads, evaporating the water to dry at 90-110 ℃, carbonizing the sample to dry dregs at 180-250 ℃, adding magnesium oxide and heating the bottom of the sample to gray or white at 300-350 ℃, ashing temperature 540 ℃ and ashing time 8 h. The recovery rate of the improved method was 100.0%-106.0%, and the relative standard deviation was 1.88%-11.78%. The improved method could accurately determine trace arsenic in vegetable oil. |
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