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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                                                                Δ


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        陈 欢   1,2* ,马 玲 ,苏晓娟 ,李艳婷 ,马 霞 ,马学琴 (1.宁夏回族自治区药品检验研究院,银川 750002;
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        2.宁夏药物创制与仿制药研究重点实验室,银川 750004;3.宁夏医科大学药学院,银川 750004)
        中图分类号 R917          文献标志码 A          文章编号 1001-0408(2022)08-0957-05
        DOI  10.6039/j.issn.1001-0408.2022.08.09

        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YMC C30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 1.0 mL/min,检测波长为 450
        nm,进样量为20 μL。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
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        量浓度的线性范围分别为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(R 均大于0.999);精密
        度、重复性、稳定性(16 h)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。
        关键词    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

        Establishment of quantitative analysis of multi-components by singer marker for content determination of
        4 carotenoids in Lycium barbarum
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        CHEN Huan ,MA Ling ,SU Xiaojuan ,LI Yanting ,MA Xia ,MA Xueqin(1. Ningxia Hui Autonomous Region
        Institute of Drug Control,Yinchuan 750002,China;2. Ningxia Key Laboratory of Drug Creation and Generic
        Drug Research,Yinchuan 750004,China;3. College of Pharmacy,Ningxia Medical University,Yinchuan 750004,
        China)
        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 C30 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 R >0.999). RSDs of precision,repeatability and
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        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.
        KEYWORDS    Lycium barbarum;HPLC;QAMS;zeaxanthin;β-carotene;β-cryptoxanthin palmitate;zeaxanthin dipalmitate


            Δ 基金项目:宁夏回族自治区重点研发计划项目(No.宁科社                      类胡萝卜素是中药枸杞子所含的主要色素,也是其
       〔2017〕13号);宁夏药物创制与仿制药研究重点实验室开放课题
                                                           重要的活性成分之一,具有提高人体免疫功能、抗肿瘤、
           *副主任药师。研究方向:药物分析。电话:0951-4104813。
                                                           抗氧化、护肝、保护视力等作用             [1-5] 。枸杞子中含有β-胡
        E-mail:233496697@qq.com
            # 通信作者:教授,博士。研究方向:药物分析。电话:0951-                萝卜素、玉米黄质等游离类胡萝卜素和玉米黄素双棕榈
        6880693。E-mail:maxueqin217@126.com                 酸酯、β-隐黄素棕榈酸酯等类胡萝卜素酯成分,其中玉


        中国药房    2022年第33卷第8期                                               China Pharmacy 2022 Vol. 33 No. 8  ·957 ·
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