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    超高效液相色谱-串联质谱法测定电子烟烟液中6种非挥发性有机酸的含量

    Determination of 6 Involatile Organic Acids in E-Liquids by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

    • 摘要: 按照题示方法测定电子烟烟液中DL-酒石酸、苹果酸、乳酸、柠檬酸、乙酰丙酸和苯甲酸等6种非挥发性有机酸的含量。取0.1 g样品,加入0.05 mL 1 g·L−1的苯甲酸-d5和丁二酸-d6混合同位素内标溶液和10 mL含0.1%(体积分数,下同)甲酸的10%(体积分数)甲醇溶液,加盖密封,涡旋振荡20 min。用0.005 g·L−1混合同位素内标溶液稀释20倍,用有机相滤膜过滤,滤液采用超高效液相色谱-串联质谱法测定。6种非挥发性有机酸在Waters HSS T3色谱柱上以不同体积比的5 mmol·L−1甲酸铵溶液(用甲酸调节其酸度至pH 2.5)和含0.1%甲酸的甲醇溶液的混合溶液(流动相)进行梯度洗脱,电喷雾离子源负离子(ESI)模式电离,多反应监测(MRM)模式检测,内标法定量。结果显示:6种非挥发性有机酸与内标的质量浓度比值均在一定范围内和对应的定量离子峰面积比值呈线性关系,检出限为0.01~0.22 mg·g−1;按照标准加入法进行回收试验,回收率为90.4%~106%,日内、日间精密度试验所得测定值的相对标准偏差(n=6)为0.60%~4.9%和1.5%~7.9%。方法用于30个实际样品的分析,6种非挥发性有机酸均有不同程度地检出,但是检出量均未超出GB 41700—2022的允许最大使用量。

       

      Abstract: Six involatile organic acids, including DL-tartrate, malic acid, lactic acid, citric acid, acetic acid, and benzoic acid, in e-liquid were determined by the method shown by the title. An aliquot (0.1 g) of sample was taken, and 0.05 mL of 1 g · L−1 mixed isotope internal standard solution of benzoic acid-d5 and succinic acid-d6, and 10 mL of 10% (volume fraction) methanol solution containing 0.1% (volume fraction, the same below) formic acid were added. After covering by a seal and shaken for 20 min by vortex, the solution was diluted 20 times by 0.005 g · L−1 mixed isotope internal standard solution, and passed through an organic phase filter membrane. The filtrate was determined by ultra-high performance liquid chromatography-tandem mass spectrometry. Six involatile organic acids were separated by gradient elution on Waters HSS T3 column with mixed solutions of 5 mmol · L−1 ammonium formate solution (adjusting its acidity to pH 2.5 with formic acid) and methanol solution containing 0.1% formic acid at different volume ratios as mobile phase, ionized in ESI mode, detected in MRM mode, and quantified by the internal standard method. It was shown that linear relationships between values of the mass concentration ratios and peak area ratios of six involatile organic acids to isotopic internal standards were kept in definite ranges, with detection limits in the range of 0.01-0.22 mg · g−1. Test for recovery was made according to the standard addition method, giving recoveries in the range of 90.4%-106%, and RSDs (n=6) of the determined values obtained from intra-day and inter-day precision tests were found in the ranges of 0.60%-4.9% and 1.5%-7.9%, respectively. The method was used for the analysis of 30 actual samples, and six involatile organic acids were detected to varying degrees, but the detected amounts did not exceed the maximum allowable amount limit of GB 41700—2022.

       

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