| 魏军晓，耿元波，岑况.炭化-湿法消解-石墨炉原子吸收光谱法测定植物油中铅、镉和铬的研究[J].中国油脂,2018,43(7):.[WEI Junxiao，GENG Yuanbo，CEN Kuang.Determination of lead, cadmium and chromium in vegetable oil by carbonization-wet digestion-graphite furnace atomic absorption spectrometry[J].China Oils and Fats,2018,43(7):.] |
| 炭化-湿法消解-石墨炉原子吸收光谱法测定植物油中铅、镉和铬的研究 |
| Determination of lead, cadmium and chromium in vegetable oil by carbonization-wet digestion-graphite furnace atomic absorption spectrometry |
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| DOI： |
| 中文关键词: 植物油 炭化 湿法消解 石墨炉原子吸收光谱法 |
| 英文关键词:vegetable oil carbonization wet digestion GFAAS |
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| 中文摘要: |
| 为了快速、准确、低成本地消解植物油，检测Pb、Cd和Cr含量，通过对比消解用酸和取样量，优化石墨炉原子吸收光谱仪（GFAAS）灰化温度和原子化温度，对比消解方法及ICP-OES、ICP-MS和GFAAS等方法的精密度，采用炭化-湿法消解-GFAAS测定了12类219件植物油(134件食用油和85件调味油)Pb、Cd和Cr含量，同时利用加标回收进行质量控制。结果表明：取样量为0.200 0 g，消解用酸为硝酸13 mL、过氧化氢5 mL时，可将植物油消解彻底；采用氘灯背景校正法测定Pb和Cd，塞曼背景校正法测定Cr；测定Pb、Cd和Cr的灰化温度和原子化温度分别为400、300、1 400?℃ 及1 100、800、2 000?℃；加标回收率范围为94.6%~109.3%；食用油Pb、Cd和Cr含量平均值为0.052 2、0.001 0、0.331 7 mg/kg，调味油的Pb、Cd和Cr含量平均值为0.192 5、0.003 7、1.813 8 mg/kg。调味油Pb、Cd和Cr的含量普遍高于食用油中的含量；炭化-湿法消解-GFAAS测定Pb、Cd和Cr的精密度较高、方法可靠，是批量检测植物油Pb、Cd和Cr的优选方法。 |
| 英文摘要: |
| For fast and accurate digestion of vegetable oil and determination of the contents of Pb, Cd and Cr in it with low cost, carbonization-wet digestion-graphite furnace atomic absorption spectrometry(GFAAS) was adopted in the determination of Pb, Cd and Cr in 219 vegetable oil samples (134 edible oil samples and 85 seasoning oil samples) of 12 types after comparing digestion acid and sample amounts, optimization ashing temperature and atomization temperature, and comparing digestion method and the RSDs of the ICP-OES, ICP-MS, and GFAAS. Quality control was also carried out in the manner of standard recovery. The results showed that vegetable oil could be completely digested under the conditions of sample amount 0.200 0 g , nitric acid 13 mL and hydrogen peroxide 5 mL. The Pb and Cd were determined using the deuterium lamp, and the Zeeman background was used to determine Cr. The optimal instrument conditions were obtained as follows: ashing temperature of Pb, Cd and Cr 400, 300, 1 400?℃ and atomization temperatures of Pb, Cd and Cr 1 100, 800, 2 000?℃. The standard recovery was in the range of 94.6%-109.3%. The average contents of Pb, Cd and Cr in edible oils were 0.052 2, 0.001 0 mg/kg and 0.331 7 mg/kg, respectively, and the average contents in seasoning oils were 0.192 5, 0.003 7 mg/kg and 1.813 8 mg/kg. The contents of Pb, Cd and Cr in seasoning oils were generally higher than those in edible oils. The carbonization-wet digestion-GFAAS had advantages of high precision and reliability in the determination of Pb, Cd and Cr and it was the preferred method for batch determination of Pb, Cd and Cr in vegetable oil. |
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