高效液相色谱分析四溴双酚A标准样品方法优化及应用
Optimization and application of HPLC method for tetrabromobisphenol A reference material analysis
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摘要: 本文通过优化液相色谱柱、流动相和波长等条件,建立了高效液相色谱分析甲醇中四溴双酚A(TBBPA)标准样品的方法.结果表明,固定相为氰基的色谱柱,在80%乙腈+20%的0.1%氨水的流动相和212 nm波长条件下,TBBPA能获得峰型最好、响应最高的色谱峰.建立的高效液相色谱分析方法,在5.0—50 μg·mL-1浓度范围内,线性和精密度均良好,检出限为0.69 μg·mL-1,满足甲醇中TBBPA标准样品分析要求.将优化的仪器分析方法用于甲醇中TBBPA标准样品的均匀性检验和稳定性研究中,结果表明,研制的甲醇中TBBPA标准样品满足均匀性要求,且在17个月内室温和4℃冷藏条件均能稳定保存.本研究建立的高效液相色谱法也可用于其他TBBPA相关样品的分析中.
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关键词:
- 四溴双酚A(TBBPA) /
- 高效液相色谱法(HPLC) /
- 方法优化 /
- 标准样品
Abstract: In this paper, a high performance liquid chromatography (HPLC) method for the determination of tetrabromobisphenol A (TBBPA) reference material (RM) in methanol was established by optimizing the kind of column, the condition of mobile phase and wavelength. The results showed that TBBPA exhibited the best peak type and the highest response under the following condition: mobile phase of 80% acetonitrile +20% 0.1% ammonia, and the wavelength of 212 nm. The established HPLC method had good linearity and precision within the concentration range of 5.0—50 μg·mL-1, and the detection limit was 0.69 μg·mL-1, which met the analysis requirements of TBBPA RM in methanol. The optimized method was used to test the homogeneity and stability of TBBPA RM in methanol. The results showed that the developed TBBPA RM was homogeneous and could be stored stably both at room temperature and 4 ℃ for 17 months. The established HPLC method in this study could also be used in the analysis of other TBBPA samples. -
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