Rapid Determination of Inorganic and Organic Iodine in Edible Salt and Kelp Samples by a Z-Ⅱ Iodine Probe
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摘要: 目前食盐和海带产品中碘含量分析主要是总碘含量测定，而无机碘与有机碘形态分析主要依靠大型精密仪器联用技术。本文研制了一种基于硫化碘化银法研制的全固态、无内参液的晶体膜电极（Z-Ⅱ碘探针），采用聚四氟乙烯消化罐微波消解技术，建立了食用盐及海带中的无机碘及有机碘含量测定方法。实验结果表明：食盐中无机碘含量为20mg/kg，有机碘含量为2mg/kg，海带中有机碘含量为2.9×103mg/kg。无机碘及有机碘含量分别在10~100mg/kg范围内线性关系良好，加标回收率为97.1%~101.0%，检出限均为1mg/kg。本方法应用于食盐和海带实际样品中的碘含量测定，无机碘和有机碘测定结果的相对标准偏差（RSD）分别小于0.92%和2.49%，且测定结果与国家标准方法和紫外分光光度法的测定结果基本一致。该方法具有试剂耗量少、成本低的特点，操作方便，可应用于有机碘和无机碘含量的测定。Abstract:
BACKGROUNDAt present, iodine content in edible salt and kelp products is mainly determined as the form of total iodine content, but the speciation analysis of inorganic iodine and organic iodine mainly relies on the hyphenated techniques of large-scale instruments. OBJECTIVESTo establish the determination method of iodine content in edible salt and kelp as well as the digestion method for the organic iodine in the closed PTFE bomb. METHODSRapid determination of inorganic and organic iodine content in edible salt and kelp products by using crystal membrane electrode technique with a solid-state and no internal reference liquid crystal film electrode (Z-Ⅱ iodine probe) developed by silver sulfide iodide method, combined with PTFE bomb microwave digestion technique. RESULTSTable salt contained 20mg/kg of inorganic iodine, and 2mg/kg of organic iodine. The concentration of organic iodine was 2.9×103mg/kg in kelp. The linear correlation of inorganic and organic iodine contents in the range of 10-100mg/kg was good. The standard-addition recoveries were 97.1%-101.0%, and the detection limit was up to 1mg/kg. This method was applied to the determination of iodine content in actual edible salt and kelp on the market, the relative standard deviation of inorganic and organic iodine in the samples was less than 0.92% and 4.20%, respectively. The analytical results were in agreement with those of the national standard method and ultraviolet spectrophotometry method, which indicated that the established method was reliable. CONCLUSIONSThe analytical method has the advantages of low reagent consumption, low cost and convenient operation, which can be used for the determination of inorganic and organic iodine contents. -
Key words:
- probe /
- rapid determination /
- organic iodine /
- inorganic iodine /
- edible salt /
- kelp
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表 1 无机碘和有机碘标准溶液工作溶液中碘含量的相关测定数据
Table 1. Determination data of iodine content in iodine standard working solution
标准溶液浓度
(mg/L)食盐样品 标准溶液浓度
(mg/L)含碘物质样品 无机碘
(mV)有机碘
(mV)高浓度有机碘
(mV)0.1 58.90 - 1 318.92 0.2 64.39 71.11 2 329.90 0.4 77.82 83.32 3 335.40 0.6 86.37 93.69 5 342.72 1.0 98.58 105.29 10 353.71 2.0 117.50 121.79 20 364.70 
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表 2 食盐中无机碘离子含量测定结果
Table 2. Analytical results of inorganic iodine contents in eatable salt samples
样品 有机碘离子含量(mg/kg) RSD
(%)本法分次测定值 平均值 加碘精制盐 19.87 19.99 20.23 20.03 0.92 低钠盐 21.41 21.20 21.22 21.28 0.77 海藻加碘食盐 19.87 20.06 20.07 20.00 0.56
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表 3 食盐和海带中有机碘离子含量测定结果
Table 3. Analytical results of organic iodine contents in eatable salt and kelp samples
样品 有机碘离子含量(mg/kg) RSD
(%)本法分次测定值 平均值 低钠盐 2.12 2.08 2.10 2.10 0.95 海藻加碘食盐 1.96 2.06 2.01 2.01 2.49 海带 2.4×103 2.9×103 3.4×103 2.9×103 -
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表 4 食盐中无机碘离子含量标准加入测定结果
Table 4. Standard results of inorganic iodine contents in eatable salt samples
样品 无机碘离子含量(mg/kg) 加标后测定值
(mg/kg)回收率
(%)碘探针法 标准方法 紫外分光光度法 加碘精制盐 20.03 20.22 18.56 30.13 101.0 低钠盐 21.28 21.26 18.39 30.99 97.1 海藻加碘食盐 20.00 - 21.94 30.01 100.1
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表 5 食盐中有机碘离子含量标准加入测定结果
Table 5. Standard results of organic iodine contents in eatable salt samples
样品 有机碘离子含量(mg/kg) 加标后测定值
(mg/kg)回收率
(%)碘探针法 标准方法 低钠盐 2.10 2.32 3.10 100.0 海藻加碘食盐 2.01 1.92 3.00 99.0
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