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    电感耦合等离子体质谱法测定巴戟天中22种元素的含量及溶出特性

    Determination of 22 Elements in Morinda Officinalis by Inductively Coupled Plasma Mass Spectrometry and Their Extraction Characteristics

    • 摘要: 取0.3 g巴戟天样品,加入硝酸7 mL,浸泡过夜,于195 ℃微波消解45 min,于100 ℃加热赶酸至1~2 mL,用5%(体积分数,下同)硝酸溶液转移至50 mL容量瓶中,加入1 mg·L−1 Au标准溶液0.2 mL,用5%硝酸溶液定容,即得元素总量供试品溶液。采用水煎煮、乙醇、仿生提取液(人工胃液和人工肠液)提取巴戟天中各元素,通过在线引入20 μg·L−1 Sc、Ge、In、Bi混合内标溶液,采用电感耦合等离子体质谱法(ICP-MS)测定上述各溶液中Be、B、Al、V、Cr、Mn、Fe、Co、Ni、Cu、Zn、As、Se、Sr、Mo、Cd、Sn、Sb、Ba、Hg、Tl、Pb等22种元素含量。分析3种提取方式下22种元素的溶出率,并采用最大限量理论值评估22种元素对人体造成的潜在健康风险。结果表明,22种元素的质量浓度在一定范围内与内标校正后的响应强度均呈线性关系,检出限(3s/k)为0.001~0.528 mg·kg−1。按照标准加入法进行回收试验,回收率为84.3%~103%,测定值的相对标准偏差(n=6)小于7.0%。柑橘叶成分分析标准物质GBW10020的测定值均在认定值的不确定度范围内。各元素的水煎煮提取溶出率、乙醇提取溶出率、仿生提取溶出率为2.35%~75.9%、0.205%~30.6%、4.18%~93.1%。方法用于分析14批样品,样品中各元素的含量虽有差异,但是元素间含量的变化趋势基本一致,样品中各元素检出量均小于对应元素的最大限量理论值,说明22种元素风险水平较低。

       

      Abstract: The Morinda officinalis sample (0.3 g) was taken, and 7 mL of nitric acid was added. The mixture was soaked overnight, dissolved by microwave digestion at 195 °C for 45 min, and heated to 1−2 mL at 100 ℃ in order to drive the acid. The solution was transferred into a 50 mL-volumetric flask with 5%(volume fraction, the same below) nitric acid solution, and 0.2 mL of 1 mg·L−1 Au standard solution was added. The solution was made its volume up to 50 mL with 5% nitric acid solution, and the total element content test solution was obtained. The various elements in Morinda officinalis were extracted by water decoction, ethanol and bionic extraction solution (artificial gastric juice and artificial intestinal juice), 20 μg·L−1 of the mixed internal standard solution of Sc, Ge, In and Bi was introduced online, and 22 elements (Be, B, Al, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Sr, Mo, Cd, Sn, Sb, Ba, Hg, Tl, and Pb) in the above solutions were determined by inductively coupled plasma mass spectrometry (ICP-MS). The extraction rates of the 22 elements under three extraction methods were analyzed, and their potential health risks to humans were assessed using the maximum theoretical limit values. As shown by the results, linear relationships between the response intensities after internal standard correction and mass concentrations of 22 elements were kept in definite ranges, with detection limits (3s/k) in the range of 0.001−0.528 mg·kg−1. Test for recovery was made by the standard addition method, giving results in the range of 84.3%−103%, with RSDs of the determined values (n=6) less than 7.0%. The determined values of the reference material GBW10020 for citrus leaf component analysis were within the uncertainty ranges of the certified values. The extraction rates of water decoction extraction, ethanol extraction and bionic extraction for elements were 2.35%−75.9%, 0.205%−30.6% and 4.18%−93.1%, respectively. This method was used to analyze 14 batches of samples. Although the contents of elements in the samples varied, the changing trends of the contents among the elements were basically the same. The detected amounts of elements in the samples were less than the maximum theoretical limit values of the corresponding elements, indicating that the risk levels of the 22 elements were relatively low.

       

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