枸杞子中4种类胡萝卜素成分含量测定一测多评法的建立
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篇名: 枸杞子中4种类胡萝卜素成分含量测定一测多评法的建立
TITLE: Establisment of quantitative analysis of multi-components by singer marker for content determination of 4 carotenoids in Lycium barbarum
摘要: 目的 建立同时测定枸杞子中玉米黄质、β-胡萝卜素、β-隐黄素棕榈酸酯、玉米黄素双棕榈酸酯含量的方法。方法枸杞子药材经正己烷-无水乙醇-丙酮-甲苯(10∶6∶7∶7,V/V/V/V)超声提取后,采用高效液相色谱法进行测定。以YMCC30为色谱柱,以甲醇-乙腈-水(81∶14∶5,V/V/V)为流动相A、二氯甲烷为流动相B进行梯度洗脱,柱温为20℃,流速为1.0mL/min,检测波长为450nm,进样量为20μL。以玉米黄质为参照物,计算β-胡萝卜素、β-隐黄素棕榈酸酯、玉米黄素双棕榈酸酯的相对校正因子,再以此计算上述成分的含量,并与外标法测定结果进行比较。结果玉米黄质、β-胡萝卜素、β-隐黄素棕榈酸酯、玉米黄素双棕榈酸酯检测质量浓度的线性范围分别为0.1194~2.9838、0.1217~1.5216、0.2859~5.7188、8.4605~211.5133μg/mL(R2均大于0.999);精密度、重复性、稳定性(16h)试验的RSD均小于4%;平均加样回收率分别为103.34%、107.37%、105.64%、96.16%(RSD<5%,n=9)。β-胡萝卜素、β-隐黄素棕榈酸酯、玉米黄素双棕榈酸酯的平均相对校正因子分别为1.109、1.390、1.158;一测多评法与外标法所测上述成分含量的相对误差均在±1%之内。结论本研究所建立的高效液相色谱法联合一测多评法准确、稳定,可用于枸杞子中4种类胡萝卜素成分的含量测定及质量控制。
ABSTRACT: OBJECTIVE To establish a method for simultaneous determination of zeaxanthin ,β-carotene,β-cryptoxanthin palmitate and zeaxanthin dipalmitate in Lycium barbarum . METHODS L. barbarum was extracted with n-hexane-anhydrous ethanol-acetone-toluene(10∶6∶7∶7,V/V/V/V)by ultrasonic method. High performance liquid chromatography (HPLC)method was adopted. The determination was performed on YMC C 30 column with mobile phase A consisted of methanol-acetonitrile-water (81∶ 14 ∶ 5,V/V/V)and mobile phase B consisted of dichloromethane (gradient elution )at the flow rate of 1.0 mL/min. The column temperature was set at 20 ℃. The detection wavelength was set at 450 nm,and sample size was 20 μL. Using zeaxanthin as control,the relative correction factors (RCFs)of β-carotene,β-cryptoxanthin palmitate and zeaxanthin dipalmitate were calculated , and then the content of each component was calculated according to RCFs and compared with the results of external standard method(ESM). RESULTS The linear range of zeaxanthin ,β-carotene,β-cryptoxanthin palmitate and zeaxanthin dipalmitate were 0.119 4-2.983 8,0.121 7-1.521 6,0.285 9-5.718 8,8.460 5-211.513 3 μg/mL(all R2>0.999). RSDs of precision ,repeatability and stability(16 h)tests were all less than 4%. The average recoveries were 103.34%,107.37%,105.64%,96.16%(RSD<5%,n= 9). The average RCFs of β-carotene,β-cryptoxanthin palmitate and zeaxanthin dipalmitate were 1.109,1.390,1.158. The relative errors of the content determination results by quantitative analysis of multi-components by singer marker (QAMS)and ESM were within ±1%. CONCLUSIONS The established HPLC-QAMS method is accurate and stable ,which can be used for the content determination and quality control of 4 carotenoids in L. barbarum .
期刊: 2022年第33卷第08期
作者: 陈欢,马玲,苏晓娟,李艳婷,马霞,马学琴
AUTHORS: CHEN Huan,MA Ling,SU Xiaojuan ,LI Yanting ,MA Xia,MA Xueqin
关键字: 枸杞子;高效液相色谱法;一测多评法;玉米黄质;β-胡萝卜素;β-隐黄素棕榈酸酯;玉米黄素双棕榈酸酯
KEYWORDS: Lycium barbarum ;HPLC;QAMS;zeaxanthin;β-carotene;β-cryptoxanthin palmitate ;zeaxanthin dipalmitate
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