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一测多评法同时测定瑶药月里瑶秘喷雾剂中 7 种有效成分的含

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        张競之 ,赵丹青 ,王正蓉 ,贾金艳 ,杨 林 ,张升盛 ,刘歆蕾 ,伍 庆 ,潘 卫 (1.贵州医科大学医学检验学
                                         3
               1*
        院,贵阳 550004;2.贵州医科大学附属医院贵州省产前诊断中心,贵阳 550004;3.贵州宏宇药业有限公司,贵阳
        550001;4.贵州师范大学贵州省山地环境信息系统与生态环境保护重点实验室/分析测试中心,贵阳 550001)
        中图分类号 R917;R29          文献标志码 A           文章编号     1001-0408(2020)09-1044-06
        DOI   10.6039/j.issn.1001-0408.2020.09.05
        摘   要   目的:建立一测多评(QAMS)法同时测定瑶药月里瑶秘喷雾剂中α-香附酮、α-蒎烯、β-蒎烯、柠檬烯、β-榄香烯、氧化石竹
        烯、藁本内酯等7种有效成分的含量,为该制剂质量控制提供方法参考。方法:采用气相色谱法进行测定。色谱柱为DB-1701P毛
        细管柱,载气为氮气,氢火焰离子检测器的温度为240 ℃,程序升温,进样口温度为240 ℃,进样量为1 μL,分流比为20∶1。以柠檬
        烯为内参物,计算其余6种成分的相对校正因子,再根据相对校正因子计算出6种成分的含量,并与内标法(以萘为内标物)测定结
        果进行比较。结果:α-香附酮、α-蒎烯、β-蒎烯、柠檬烯、β-榄香烯、氧化石竹烯、藁本内酯检测质量浓度的线性范围分别为0.008 9~
        1.110 0、0.028 3~3.540 0、0.020 5~2.560 0、0.023 0~2.880 0、0.016 3~2.035 0、0.013 1~1.640 0、0.008 3~1.040 0 mg/mL(r 均大
        于0.999 0);定量限分别为0.005 6、0.013 1、0.011 4、0.018 6、0.010 8、0.008 9、0.004 5 mg/mL;检测限分别为0.001 9、0.004 1、0.003 7、
        0.006 2、0.003 5、0.002 9、0.001 5 mg/mL;精密度、稳定性(24 h)、重复性试验的RSD均小于2%(n=5或n=6);平均回收率分别为
        98.48%、101.37%、97.96%、99.80%、102.79%、97.77%、102.14%,RSD均小于2%(n=9)。α-香附酮、α-蒎烯、β-蒎烯、β-榄香烯、氧
        化石竹烯、藁本内酯的平均相对校正因子分别为 1.045 8、0.621 0、0.488 5、0.382 9、0.708 9、0.956 9,RSD 均小于 2%(n=6)。QA-
        MS法和内标法测得的7种成分的含量差异均无统计学意义(P>0.05)。结论:建立的QAMS法简便、准确、稳定且重现性良好,可
        用于月里瑶秘喷雾剂中7种成分的同时测定。
        关键词 一测多评法;瑶药;月里瑶秘喷雾剂;气相色谱法;质量控制
        Simultaneous Determination of 7 Effective Components in Yao Medicine Yueli Yaomi Spray by QAMS
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        ZHANG Jingzhi ,ZHAO Danqing ,WANG Zhengrong ,JIA Jinyan ,YANG Lin ,ZHANG Shengsheng ,LIU
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        Xinlei ,WU Qing ,PAN Wei (1.School of Clinical Laboratory Science,Guizhou Medical University,Guiyang
                                  1,2
        550004,China;2.Guizhou Provincial Prenatal Diagnosis Center,the Affiliated Hospital of Guizhou Medical
        University,Guiyang 550004,China;3.Guizhou Hongyu Pharmaceutical Co.,Ltd.,Guiyang 550001,China;4.
        Guizhou Key Laboratory of Mountainous Environment Information System and Environment Protection/Analysis
        and Measurement Center,Guizhou Normal University,Guiyang 550001,China)
        ABSTRACT    OBJECTIVE:To establish QAMS method for simultaneous determination of 7 effective components in Yao
        medicine Yueli yaomi spray,such as α-cyperone,α-pinene,β-pinene,limonene,β-elemene,caryophyllene oxide and ligustilide,
        so as to provide method reference for the quality control of the preparation. METHODS:GC method was adopted. The
        determination was performed on DB-1701P capillary column,using nitrogen as carrier gas. The temperature of the hydrogen flame
        ion detector was 240 ℃. The temperature was programmed,the inlet temperature was 240 ℃,the injection volume was 1 μL and
        the split ratio was 20 ∶ 1. Using limonene as internal reference,the relative correction factors of other 6 components were
        calculated,the contents of them were calculated with relative correction factors,and then compared with the results of internal
        standard method (using naphthalene as internal standard). RESULTS:The mass concentration linear range of α-cyperone,
        α-pinene,β-pinene,limonene,β-elemene,caryophyllene oxide and ligustilide were 0.008 9-1.110 0,0.028 3-3.540 0,0.020 5-
        2.560 0,0.023 0-2.880 0,0.016 3-2.035 0,0.013 1-1.640 0,0.008 3-1.040 0 mg/mL(all r>0.999 0);the limits of quantification
        were 0.005 6,0.013 1,0.011 4,0.018 6,0.010 8,0.008 9,0.004 5 mg/mL;the detection limits were 0.001 9,0.004 1,0.003 7,
        0.006 2,0.003 5,0.002 9,0.001 5 mg/mL;RSDs for precision,stability(24 h),and repeatability tests were all less than 2%
                                                           (n=5 or n=6); the average recoveries were 98.48% ,
            Δ 基金项目:国家自然科学基金资助项目(No.81960284);贵州省
                                                            101.37%,97.96%,99.80%,102.79%,97.77%,102.14%,
        教育厅创新群体重大研究项目(No.黔教合KY字〔2018〕014)
            *硕士研究生。研究方向:临床检验诊断学、产前诊断。电话:                    and RSDs were all lower than 2%(n=9),respectively. The
        0851-86772684。E-mail:895264190@qq.com               average relative correction factors of α-cyperone,α-pinene,
            # 通信作者:教授,博士生导师。研究方向:临床检验诊断学、产                  β-pinene,β-elemene,caryophyllene oxide and ligustilide were
        前诊断。电话:0851-86772684。E-mail:pw_6602@sina.com        1.045 8, 0.621 0, 0.488 5, 0.382 9, 0.708 9, 0.956 9


        ·1044  ·  China Pharmacy 2020 Vol. 31 No. 9                                  中国药房    2020年第31卷第9期
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