摘要
目的建立保健食品中左旋肉碱的固相萃取净化-高效液相色谱分析方法。方法样品经10 mmol/L盐酸溶液溶解并稀释,MCX混合型阳离子固相萃取柱净化,采用ZORBAX SB-AQ C_(18)(250 mm×4.6 mm,5μm)色谱柱分离,以磷酸盐缓冲溶液(0.05 mol/L磷酸氢二钾-0.002 mol/L辛烷磺酸钠,用磷酸调pH至2.5)-乙腈=98:2为流动相,流速1.0 ml/min,紫外检测器进行检测,检测波长:210 nm,柱温:30℃,以保留时间定性,外标法定量。结果供试品溶液经净化后,与目标化合物不能基线分离的干扰物得到有效去除,左旋肉碱的质量浓度在52.35~418.80μg/ml范围内与峰面积呈良好线性关系,相关系数(r)为0.9996,平均回收率为91.71%,RSD为2.78%。结论该方法科学可靠、重复性好,可作为保健食品中左旋肉碱含量测定的方法。
Objective To establish a method for determination of L-carnitine in health food by solid phase extraction and high performance liquid chromatography.Methods The samples were dissolved and diluted with 10 mmol/L hydrochloric acid solution,and purified by MCX mixed cationic solid phase extraction column,then were separated by ZORBAX SB-AQ C_(18)(250 mm×4.6 mm,5μm)column,using phosphate buffer solution(consisted of 0.05 mol/L dipotassium phosphate and 0.002 mol/L sodium octane sulfonate adjusted to pH 2.5 with phosphoric acid)-acetonitrile=98:2 as the mobile phase.The flow rate was 1.0 ml/min,the detection was carried out by UV detector,the detection wavelength was set at 210 nm,and the column temperature was 30℃.The qualitative analysis was performed based on retention time,and the quantitative analysis was carried out through external standard method.Results After the sample solution was purified,the interfering substances that could not be separated from the target compound at baseline were effectively removed.The peak area showed a good linear relationship with the mass concentration of L-carnitine in the range of 52.35-418.80μg/ml,and the correlation coefficient(r)was 0.9996.The average recovery was 91.71%,with RSD of 2.78%.Conclusion The method is reliable,reproducible and can be used for the determination of L-carnitine in health food.
作者
李海霞
杨黎
谭宝金
刘星
文丽
LI Hai-xia;YANG Li;TAN Bao-jin;LIU Xing;WEN Li(Guangxi-Asean Food Inspection and Testing Center,Nanning 530029,China;Nanning University,Nanning 530299,China;Guangxi Zhuang Autonomous Region Food and Drug Evaluation and Inspection Center,Nanning 530029,China)
出处
《食品与药品》
CAS
2024年第6期566-569,共4页
Food and Drug
关键词
保健食品
左旋肉碱
固相萃取
高效液相色谱法
health food
L-carnitine
solid phase extraction(SPE)
high performance liquid chromatography(HPLC)
