Comparison of three methods of detecting aluminum content in jellyfish products
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摘要: 文章采用电感耦合等离子体质谱法 (ICP-MS)、分光光度法和乙二胺四乙酸 (EDTA) 滴定法测定海蜇 (Rhopilema esculentum) 产品中的铝 (Al) 含量，对比检测结果、精密度和准确度差异，分析这3种方法在产业上应用的优缺点，并采用ICP-MS对中国10个沿海城市的即食海蜇产品进行了Al残留风险摸底调查。结果表明，ICP-MS和分光光度法的测定结果差异不显著，EDTA滴定法与其他2种方法存在差异，但总体相差不大。3种测定方法对盐渍海蜇和即食海蜇样品的相对标准偏差 (Relative standard deviation, RSD) 介于1.79%~4.34%。ICP-MS对于盐渍海蜇和即食海蜇的加标回收率分别介于92%~104%和97%~100%，而分光光度法的加标回收率分别介于97%~102%和98%~101%，EDTA滴定法的加标回收率介于94%~99%，相对偏低。3种方法均符合检测要求，可根据实际需求选择合适的检测方法。此外还发现部分地区的即食海蜇Al残留量接近国家规定的限量标准。Abstract: In this paper, the content of aluminum in jellyfish (Rhopilema esculentum) was determined by inductively coupled plasma mass spectrometry (ICP-MS), spectrophotometry and EDTA titration. The differences of detection results, precision and accuracy were compared, and the advantages and disadvantages of three methods in industrial application were analyzed. The aluminum residue risk of ready-to-eat jellyfish in ten coastal cities of China was investigated by ICP-MS. The results show that there was no significant difference between ICP-MS and spectrophotometry. EDTA titration was different from the other two methods, but the difference was not significant. The relative standard deviation (RSD) of the three methods for salted jellyfish and ready-to-eat jellyfish ranged from 1.79% to 4.34%. The RSD of salted jellyfish and ready-to-eat jellyfish by ICP-MS were 92%−104% and 97%−100%, respectively. The RSD of spectrophotometry were 97%−102% and 98%−101%, respectively. The recovery of EDTA titration was 94%−99%, which were relatively low. The three methods all meet the testing requirements, and the appropriate testing method can be selected according to the actual needs. The results also indicate that the Al residue in ready-to-eat jellyfish in some areas is close to the national limit.
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Keywords:
- Jellyfish /
- Aluminum /
- ICP-MS /
- Spectrophotometry /
- EDTA titration method
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图 1 3种方法测定盐渍、即食海蜇铝质量分数对比
a. 3种方法测定盐渍海蜇中铝质量分数对比；b. 3种方法测定即食海蜇中铝质量分数对比。
Figure 1. Comparison of three methods to determine Al content in salted jellyfish and ready-to-eat jellyfish
a. Comparison of three methods to determine Al content in salted jellyfish; b. Comparison of three methods to determine Al content in ready-to-eat jellyfish.
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图 2 3种方法加标回收率比较
a、b分别为盐渍海蜇和即食海蜇ICP-MS的加标回收率；c、d分别为盐渍海蜇和即食海蜇分光光度法的加标回收率；e、f 分别为盐渍海蜇和即食海蜇EDTA滴定法的加标回收率。
Figure 2. Comparison of spiked recovery rates of three methods
a, b. Spiked recovery rates of salted jellyfish and ready-to-eat jellyfish by ICP-MS, respectively; c, d. Spiked recovery rates of salted jellyfish and ready-to-eat jellyfish by spectrophotometry, respectively; e, f. Spiked recovery rates of salted jellyfish and ready-to-eat jellyfish by EDTA titration, respectively.
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图 3 市售即食海蜇样品普查
*. 同一省份不同市即食海蜇的铝质量分数有差异(P<0.05)；**. 差异显著 (P<0.01)；***. 差异极显著(P<0.001)。
Figure 3. Survey of ready-to-eat jellyfish samples in market
*.The aluminum mass fraction in ready-to-eat jellyfish between different cities in the same province is different (P<0.05); **. Significant difference (P<0.01); ***. Very significant difference (P<0.001).
表 1 微波消解仪消解条件
Table 1 Digestion conditions of microwave digestion apparatus
步骤
Step功率
Power/W温度
Temperature/℃升温时间
Heating time/min保持时间
Hold time/min1 1 200 120 10 3 2 1 200 160 5 5 3 1 200 180 5 20 
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表 2 ICP-MS仪器条件
Table 2 ICP-MS instrument conditions
项目 Item 参数 Parameter 项目 Item 参数 Parameter 射频功率 Radio-frequency power/W 1550 雾化器 Nebulizer 同心雾化器 矩管 Rectangular tube 石英管，2.5 mm中心通道 雾化室 Spray chamber 石英双通道 采样锥/截取锥 Sampling cone/Skimmer cone 1.0/0.4 mm镍锥 等离子气体流量 Plasma gas flow rate/(L·min−1) 15.0 载气流量 Carrier gas flux/(L·min−1) 1.0 辅助气流量 Auxiliary gas flow/(L·min−1) 1.0 提升速度 Sample lifting rate/(r·s−1) 45 稳定时间 Stability time/s 45 采样深度 Sample depth/m 8 样品提升速度 Sample lifting rate/(r·s−1) 0.1 雾化室温度 Atomizing chamber temperature/℃ 2 每峰测定点数 Measure points per peak 3
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表 3 3种检测方法精密度比较
Table 3 Comparison of precision of three detection methods
方法
Method样品
Sample铝质量分数
Aluminum mass fraction/(mg·kg−1)平均值
Average/(mg·kg−1)标准差
SD/%相对标准差
RSD/%ICP-MS 盐渍 539.60 539.26 531.26 530.81 538.60 546.50 537.67 5.89 2.40 即食 458.63 459.47 470.47 466.53 473.00 468.22 466.05 5.85 2.39 分光光度法
Spectrophotometric method盐渍 533.21 525.49 540.85 546.99 529.11 526.74 533.73 8.54 3.49 即食 432.59 438.73 487.87 442.57 427.98 431.82 436.93 7.48 3.05 乙二胺四乙酸滴定法
EDTA titration method盐渍 525.40 513.00 535.90 527.60 539.40 541.30 530.43 10.64 4.34 即食 425.40 429.30 434.70 422.55 427.95 432.00 428.65 4.39 1.79
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