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作 者:张舟艺[1] 张国梅 郑秋岚[1] 徐水祥[1] 孙丽华[1]
出 处:《中国卫生检验杂志》2017年第24期3541-3542,3550,共3页Chinese Journal of Health Laboratory Technology
基 金:浙江省科技厅院所专项项目(2016F10002)
摘 要:目的建立保健食品中水飞蓟宾和五味子醇甲的高效液相色谱测定方法。方法样品经甲醇超声提取,被测物采用Poroshell 120 EC-C18(4.6 mm×100 mm,2.7μm)分离柱;流动相为甲醇-水,梯度洗脱,流速为0.7 ml/min;水飞蓟宾和五味子醇甲的紫外检测波长分别为287 nm和250 nm。根据保留时间定性,外标峰面积法定量。结果水飞蓟宾在0μg/ml^243.9μg/ml线性相关系数为0.999 7,方法检出限为1.82μg/ml,相对标准偏差(RSD)为0.84%(n=6),样品的加标回收率为97.4%~102.1%;五味子醇甲在0μg/ml^43.3μg/ml线性相关系数为0.999 6,方法检出限为0.48μg/ml,相对标准偏差(RSD)为0.56%(n=6),样品的加标回收率为97.4%~102.5%。结论该方法简单、快速、灵敏和准确,可用于保健食品中水飞蓟宾和五味子醇甲的测定。Objective To establish a method for simultaneous determination of silybin and schisandrin in health food by high performance liquid chromatography( HPLC). Methods The samples were extracted by ultrasonic extraction by methanol,target chemicals in samples were ultrasonically extracted with methanol and then were separated on Poroshell 120 EC-C18( 4. 6 mm ×100 mm,2. 7 μm). The mobile phase solution of methanol-water was used at a flow rate of 0. 7 ml/min. The UV detection wavelengths of silybin was 287 nm and schizandrin was 250 nm. Qualification was conducted according to the retention time,and the external standard peak area was used for quantification. Results When the concentration of silybin was within 0. 0 μg/ml-243. 9 μg/ml,the correlation coefficient was 0. 999 7,the detection limit of the method was 1. 82 μg/ml,the relative standard deviation( RSD) was 0. 84%( n = 6),and the recoveries of samples were within 97. 4%-102. 1%. When the concentration of schizandrin was within 0. 0 μg/ml-43. 3 μg/ml,the correlation coefficient was 0. 999 6,the detection limit of the method was0. 48 μg/ml,the relative standard deviation( RSD) was 0. 56%( n = 6),and the recoveries of samples were within 97. 4%-102. 5%. Conclusion The method is simple,fast,sensitive and accurate,and it is suitable to the determination of silybin and schisandrin in health food.
分 类 号:R155.5[医药卫生—营养与食品卫生学]
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