优化毛细管气相色谱法测定保健品中维生素E的含量
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摘要
目的:优化毛细管气相色谱法色谱参数并用于测定各种类型保健品中维生素E的含量。方法:优化气相色谱法的进样口分流比、气化温度、升温程序等参数,进样口分流比为25∶1;进样口温度为290℃;升温程序为200℃保持0 min,5℃·min~(-1)升到300℃,保持8 min,获得良好的分离度和色谱峰形,符合定量要求。并对比高效液相色谱法测得的维生素E含量。结果:维生素E标准曲线在0.2~2.3 mg·ml~(-1)之间线性关系良好,r=0.999 9;加样回收率为97.26%,RSD为1.71%(n=9);优化后的方法与高效液相色谱法测得的维生素E含量无明显差异。结论:优化毛细管气相色谱法适用于测定不同类型不同规格的保健品中维生素E含量,测得结果准确,方法灵敏,操作简便,同时提示目前市场上含维生素E的保健食品维生素E含量差异大,在实际使用中指导不够明确,需要引起关注。
Objective: To optimize the method parameters of capillary gas chromatography and determine the content of vitamin E in various types of health products. Methods: The optimized parameters of capillary gas chromatography were as follows: the inlet separation flow ratio was 25 ∶ 1,the inlet temperature was 290℃,the temperature programming started at 200℃,rose to 300 ℃ at 5℃ ·min~(-1) and kept for 8 min. The result obtained good separation degree and peak shape,which met the quantitative requirements. The result of vitamin E content in health products measured by capillary gas chromatography was compared with that by high performance liquid chromatography. Results: Good linearity was presented within the vitamin E concentration range of 0. 2-2. 3 mg · ml~(-1)( r =0. 999 9). The recovery rate was 97. 26% with the RSD of 1. 71%( n = 9). There was no significant difference in the content of vitamin E measured by the optimized capillary gas chromatography method and the high performance liquid chromatography method. Conclusion: The optimized capillary gas chromatography method is suitable for the content determination of vitamin E in health products with different types and specifications. The measured result is accurate and the method is sensitive and simple. It is suggested that there is obvious difference in the content of vitamin E in the marketed health products containing vitamin E,and the guidance is not clear enough for actual use and needs to be paid attention.
Objective: To optimize the method parameters of capillary gas chromatography and determine the content of vitamin E in various types of health products. Methods: The optimized parameters of capillary gas chromatography were as follows: the inlet separation flow ratio was 25 ∶ 1,the inlet temperature was 290℃,the temperature programming started at 200℃,rose to 300 ℃ at 5℃ ·min~(-1) and kept for 8 min. The result obtained good separation degree and peak shape,which met the quantitative requirements. The result of vitamin E content in health products measured by capillary gas chromatography was compared with that by high performance liquid chromatography. Results: Good linearity was presented within the vitamin E concentration range of 0. 2-2. 3 mg · ml~(-1)( r =0. 999 9). The recovery rate was 97. 26% with the RSD of 1. 71%( n = 9). There was no significant difference in the content of vitamin E measured by the optimized capillary gas chromatography method and the high performance liquid chromatography method. Conclusion: The optimized capillary gas chromatography method is suitable for the content determination of vitamin E in health products with different types and specifications. The measured result is accurate and the method is sensitive and simple. It is suggested that there is obvious difference in the content of vitamin E in the marketed health products containing vitamin E,and the guidance is not clear enough for actual use and needs to be paid attention.
引文
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9 赵孔祥,娄婷婷,何佳,等.同位素稀释/液相色谱-串联质谱测定婴幼儿配方奶粉中脂溶性维生素[J].分析测试学报,2015,34(12):1372-1376
10 蒋彦飞,张治军,钟名诚.保健食品中维生素E类成分的检测与质量评价[J].首都食品与医药,2016,23(16):24-27
2 王晓敏,李昌蝶,王继鑫,等.保健食品天然维生素E胶囊质量考察研究[J].云南师范大学学报(自然科学版),2015,35(3):70-74
3 梁诚.天然维生素E生产现状与应用前景[J].化学工业,2002,20(4):26-29
4 李利军,钟招亨,陈其锋,等.流动注射化学发光抑制法测定维生素E[J].分析试验室,2006,25(9):107-111
5 张洪,马俊玲.二阶导数分光光度法测定维生素E霜的含量[J].广东药学院学报,2000,16(2):112-114
6 中国药典[S].2015年版.二部.1242-1244
7 中华人民共和国国家标准.食品中维生素A和维生素E的测定[S].GB/T 5009.82
8 郑小锋,陈家香,余春梅,等.采用HPLC法测定维生素EC片中维生素E的含量[J].科技视界,2012,(31):292-293
9 赵孔祥,娄婷婷,何佳,等.同位素稀释/液相色谱-串联质谱测定婴幼儿配方奶粉中脂溶性维生素[J].分析测试学报,2015,34(12):1372-1376
10 蒋彦飞,张治军,钟名诚.保健食品中维生素E类成分的检测与质量评价[J].首都食品与医药,2016,23(16):24-27