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    电感耦合等离子体质谱法测定药用玻璃安瓿的多基质提取液中39种金属元素的含量

    Determination of 39 Metal Elements in Multiple Matrix Extraction Solutions of Pharmaceutical Glass Ampoules by Inductively Coupled Plasma Mass Spectrometry

      摘要
    • 摘要: 为实现药用玻璃安瓿的多基质提取液中多种金属元素的同时测定，以0.9%（质量分数，下同）氯化钾溶液、0.1 mol·L−1氢氧化钠溶液、3%（质量分数，下同）枸橼酸钠溶液、20 mmol·L−1甘氨酸溶液为模拟提取剂，进行了题示研究。药用玻璃安瓿用水洗净、晾干后，分别加入上述4种模拟提取剂，并分别于121，121，80，50 ℃加热2，2，24，24 h。移取1.0 mL模拟提取液，用8%（体积分数）王水（体积比3∶1的盐酸-硝酸混合溶液）溶液稀释至50 mL，摇匀后采用电感耦合等离子体质谱法检测，通过稀释模拟提取液和在线加入内标两种方式降低基质干扰，利用氦气碰撞模式联合干扰校正方程（仅针对铟元素）消除质谱干扰。结果表明，39种金属元素的质量浓度在一定范围内和对应的信号强度与内标信号强度的比值呈线性关系，检出限为0.000 024~0.27 mg·L−1；4种模拟提取液中39种金属元素的回收率为80.3%~112%，测定值的相对标准偏差（n=6）为0.10%~7.7%。方法用于10组药用玻璃安瓿的测定，有9种金属元素被不同程度检出，4种模拟提取剂的提取能力由大到小分别为0.1 mol·L−1氢氧化钠溶液、3%枸橼酸钠溶液、0.9%氯化钾溶液、20 mmol·L−1甘氨酸溶液。

       

      Abstract: To achieve the simultaneous determination of multiple metal elements in multiple matrix extraction solutions of pharmaceutical glass ampoules, the study mentioned by the title was conducted using the following simulated extractants: 0.9% (mass fraction, the same below) potassium chloride solution, 0.1 mol · L-1 sodium hydroxide solution, 3% (mass fraction, the same below) sodium citrate solution, and 20 mmol · L-1 glycine solution. Pharmaceutical glass ampoules were washed with water and dried, and the 4 simulated extractants were added separately. After heating at 121, 121, 80, 50 ℃ for 2, 2, 24, 24 h separately, an aliquot (1.0 mL) of the simulated extraction solution was taken and diluted to 50 mL with 8% (volume fraction)aqua regia (mixture of hydrochloric acid and nitric acid at volume ratio of 3∶1) solution. The solution obtained was mixed well, and analyzed using inductively coupled plasma mass spectrometry. Matrix interference was reduced by diluting the simulated extraction solutions and online addition of internal standards, while mass spectrometry interference was eliminated using helium collision mode combined with an interference correction equation (specifically for indium element). It was shown that the mass concentrations of the 39 metal elements exhibited linear relationships with the ratios of their signal intensities to internal standard signal intensities within definite ranges, with detection limits in the range of 0.000 024-0.27 mg · L-1. Recoveries of the 39 metal elements in the 4 simulated extraction solutions ranged from 80.3% to 112%, with RSDs (n=6) of the determined values in the range of 0.10%-7.7%. The proposed method was applied to the analysis of 10 sets of pharmaceutical glass ampoules, and 9 metal elements were detected at varying levels. The extraction capabilities of the 4 simulated extractants, ranked from highest to lowest, were: 0.1 mol · L-1 sodium hydroxide solution, 3% sodium citrate solution, 0.9% potassium chloride solution, and 20 mmol · L-1 glycine solution.

       

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