一测多评法同时测定瑶药月里瑶秘喷雾剂中7种有效成分的含量
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篇名: 一测多评法同时测定瑶药月里瑶秘喷雾剂中7种有效成分的含量
TITLE: Simultaneous Determination of 7 Effective Components in Yao Medicine Yueli Yaomi Spray by QAMS
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1μL,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0.0089~1.1100、0.0283~3.5400、0.0205~2.5600、0.0230~2.8800、0.0163~2.0350、0.0131~1.6400、0.0083~1.0400mg/mL(r均大于0.9990);定量限分别为0.0056、0.0131、0.0114、0.0186、0.0108、0.0089、0.0045mg/mL;检测限分别为0.0019、0.0041、0.0037、0.0062、0.0035、0.0029、0.0015mg/mL;精密度、稳定性(24h)、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1.0458、0.6210、0.4885、0.3829、0.7089、0.9569,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。
ABSTRACT: OBJECTIVE:To establish QAMS method for simultaneou s 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% , 014) 101.37%,97.96%,99.80%,102.79%,97.77%,102.14%, and RSDs were all lower than 2%(n=9),respectively. The average relative correction factors of α-cyperone,α-pinene, β-pinene,β-elemene,caryophyllene oxide and ligustilide were 1.045 8,0.621 0,0.488 5,0.382 9,0.708 9,0.956 9 respectively,and the RSDs were all lower than 2%(n=6). There wa s no statistical significance in contents of 7 components between QAMS method and internal standard method (P>0.05). CONCLUSIONS :The established QAMS method is simple , accurate,stable and reproducible ,and can be used for simultaneous determination for 7 components in Yueli yaomi spray.
期刊: 2020年第31卷第09期
作者: 张競之,赵丹青,王正蓉,贾金艳,杨林,张升盛,刘歆蕾,伍庆,潘卫
AUTHORS: ZHANG Jingzhi,ZHAO Danqing,WANG Zhengrong,JIA Jinyan,YANG Lin,ZHANG Shengsheng,LIU Xinlei,WU Qing,PAN Wei
关键字: 一测多评法;瑶药;月里瑶秘喷雾剂;气相色谱法;质量控制
KEYWORDS: QAMS;Yao medicine ;Yueli yaomi spray ;GC;Quality control
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