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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

量 Δ

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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