龟甲及龟甲胶中25种金属及有害元素含量测定及初步风险评估

目的：分析研究龟甲及龟甲胶中25种金属及有害元素的含量，对其进行风险评估，为质量保证提供依据。方法：采用电感耦合等离子体质谱（ICP-MS）法测定20种微量元素含量，射频功率1 200 W，雾化气流速1.04 L·min^-1，辅助气流速1.3 L·min^-1，等离子体气流速15 L·min^-1，蠕动泵20.0 r·min^-1，重复次数3次，扫描次数10次；采用火焰原子吸收光谱（FAAS）法测定5种常量元素含量，锌（Zn）、镁（Mg）、铁（Fe）、锶（Sr）、钙（Ca）的波长分别是213.8、279.6、248.3、460.7、422.7 nm，Zn、Mg、Fe、Ca的灯电流为5.0 mA，Sr的为3.0 mA，光谱通带均为0.2 nm；分析各元素间相关性。根据风险评估要求，对龟甲及龟甲胶中金属及有害元素安全性进行评估。结果：镉（Cd）、铍（Be）、银（Ag）、汞（Hg）、钛（Ti）、镝（Dy）、钯（Pd）、硒（Se）8种元素在龟甲中未检出。龟甲制成龟甲胶后金属及有害元素含量大幅降低。23批龟甲中有3批的砷（As）、铅（Pb）实际测定值（含量范围分别为0.3~1.5和1.1~1.3 mg·kg^-1）大于最大残留限量值，15批龟甲胶中的Pb、As、Hg、Cd、铜（Cu）实际测定值（含量范围分别为0~0.23、0~0.18、0~0.005、0~0.01和0~0.59 mg·kg^-1）均远小于最大残留限量值。结论：龟甲中As、Pb存在一定风险，龟甲胶中的金属及有害元素安全风险较低。

Objective:To analyze the contents of 25 metals and harmful elements in Testudinis Carapax et Plastrum and Testudinis Carapax et Plastri Colla, and to perform the risk evaluation in order to provide reference for quality assurance.Methods:The contents of 20 trace elements were determined by inductively coupled plasma mass spectrometry (ICP-MS) and the parameters of the instrument were as follows:radio frequency power:1 200 W, atomizing gas flow rate:1.04 L·min^-1, auxiliary gas flow rate:1.3 L·min^-1, plasma gas flow:15.0 L·min^-1, peristaltic pump:20.0 r·min^-1, repeat times:3 times, and scanning times:10 times.The contents of 5 macro elements were determined by flame atomic absorption spectroscopy (FAAS) with wavelengths of Zn, Mg, Fe, Sr, Ca at 213.8 nm, 279.6 nm, 248.3 nm, 460.7 nm and 422.7 nm, respectively.The lamp currents of Zn, Mg, Fe, and Ca were 5.0 mA, and that of Sr was 3.0 mA.The spectral passband was 0.2 nm.The correlations between elements were analyzed.According to the risk assessment requirements, the safety of metals and harmful elements in Ttestudinis Carapax et Plastrum and Testudinis Carapax et Plastri Colla was evaluated.Results:Cd, Be, Ag, Hg, Ti, Dy, Pd and Se were not detected in Testudinis Carapax et Plastrum.The contents of metals and harmful elements were greatly reduced in Testudinis Carapax et Plastri Colla.The contents of As and Pb in 3 batches of Testudinis Carapax et Plastrum exceeded the maximum residue limits with contents range of 0.3-1.5 mg·kg^-1 and 1.1-1.3 mg·kg^-1, respectively.The contents of Pb, As, Hg, Cd and Cu in 15 batches of Testudinis Carapax et Plastri Colla were all far below the maximum residue limits with content ranges of 0-0.23 mg·kg^-1, 0-0.18 mg·kg^-1, 0-0.005 mg·kg^-1, 0-0.01 mg·kg^-1 and 0-0.59 mg·kg^-11, respectively.Conclusion:Risks of As and Pb residues are existed in Testudinis Carapax et Plastrum, and there are no risks of metals and harmful elements residues in Testudinis Carapax et Plastri Colla.

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