Page 77 - 2019年8月第30卷第16期

一测多评法同时测定咽炎片中5种指标性成分的含量 Δ

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马昌豪 ，李怀伟，仝桂平，马海春，冯思腾（菏泽市食品药品检验检测研究院，山东 菏泽 274000）

中图分类号 R917 文献标志码 A 文章编号 1001-0408（2019）16-2232-05
DOI 10.6039/j.issn.1001-0408.2019.16.14

摘 要 目的：建立一测多评法同时测定咽炎片中芍药苷、芦丁、木蝴蝶苷B、黄芩苷、肉桂酸等5种指标性成分的含量。方法：采
用高效液相色谱法。色谱柱为Hypersil GOLD-C18 （250 mm×4.6 mm，5 μm），流动相为甲醇-0.35％磷酸水溶液（梯度洗脱），检测波
长为280 nm（芦丁、木蝴蝶苷B、黄芩苷、肉桂酸）、230 nm（芍药苷），柱温为30 ℃，流速为1 mL/min，进样量为10 μL。以芍药苷为
内参物，建立芦丁、木蝴蝶苷B、黄芩苷、肉桂酸的相对校正因子；考察不同色谱系统、色谱柱、流动相比例、流速、柱温对相对校正
因子的影响，并按相对保留时间对待测成分进行色谱峰定位。按外标法测定内参物芍药苷含量，按一测多评法测定其余4种成分
含量，并与外标法测定结果进行比较。结果：各待测成分的分离度均大于1.5；芍药苷、芦丁、木蝴蝶苷B、黄芩苷、肉桂酸的质量浓
度分别在3.97～119.22、1.96～58.68、2.39～71.64、1.92～57.51、0.54～16.24 μg/mL范围内线性关系良好（r≥0.999 7）；精密度、重复
性、稳定性试验的RSD均小于2％；平均加样回收率为97.20％～98.07％（RSD＜3％，n＝6）。以芍药苷为内参物，芦丁、木蝴蝶苷
B、黄芩苷、肉桂酸的平均相对校正因子分别为0.554 6、1.815 6、2.489 3、5.423 2；在不同色谱条件下其相对校正因子和相对保留时
间的RSD均小于5％。采用一测多评法与外标法分别测得10批咽炎片待检样品中4种成分（除内参物外）含量的相对误差绝对值
均小于1％，两种方法测定结果一致。结论：本方法准确、快捷、高效、价廉，可用于同时测定咽炎片中5种指标性成分的含量。
关键词 咽炎片；一测多评法；芍药苷；芦丁；木蝴蝶苷B；黄芩苷；肉桂酸；高效液相色谱法；含量测定

Simultaneous Determination of the Contents of 5 Indicator Components in Yanyan Tablets by QAMS
MA Changhao，LI Huaiwei，TONG Guiping，MA Haichun，FENG Siteng（Heze Institute for Food and Drug
Control，Shandong Heze 274000，China）

ABSTRACT OBJECTIVE：To establish QAMS method for content determination of paeoniflorin，rutin，oroxin B，baicalin and
cinnamates in Yanyan tablets. METHODS：HPLC method was adopted. The determination was performed on Hypersil GOLD-C18
column（250 mm×4.6 mm，5 μm）with mobile phase consisted of methanol-0.35％ phosphoric acid solution（gradient elution）at
flow rate of 1 mL/min. The detection wavelengths were set at 280 nm （rutin，oroxin B，baicalin，cinnamates） and 230 nm
（paeoniflorin）. The column temperature was 30 ℃，and sample size was 10 μL. Using paeoniflorin as internal reference，relative
correction factors（RCF）of rutin，oroxin B，baicalin and cinnamates were established. Effects of different chromatogram system，
chromatogram column，mobile phase proportion，flow rate and column temperature on relative correction factors were investigated；
the chromatographic peaks of the components were located according to the relative retention time. The content of paeoniflorin as
internal reference was determined by external standard method，and the other four components were determined by QAMS，and
then compared with the results of external standard method. RESULTS：The separation degree of each component to be measured
was greater than 1.5. The linear range was 3.97-119.22 μg/mL for paeoniflorin，1.96-58.68 μg/mL for rutin，2.39-71.64 μg/mL for
oroxin B，1.92-57.51 μ g/mL for baicalin，0.54-16.24 μ g/mL for cinnamates（r≥0.999 7），respectively. RSDs of precision，
reproducibility and stability tests were all lower than 2％. Average recoveries were 97.20％-98.07％（RSD＜3％，n＝6）. RCFs of
rutin，oroxin B，baicalin and cinnamates were 0.554 6，1.815 6，2.489 3 and 5.423 2，using paeoniflorin as internal reference. RSDs
of RCF and relative retention time were all lower than 5％ under different chromatogram conditions. Absolut relative error of four
components（except for internal reference）in 10 batches of Yanyan tablets sampled by QAMS and external standard method were
all less than 1％ . The results of the two methods were identical. CONCLUSIONS：The established method is accurate，rapid，
efficient and inexpensive，and it can be used for simultaneous determination of 5 indicator components in Yanyan tablet.
KEY WORDS Yanyan tablet；QAMS；Paeoniflorin；Rutin；Oroxin B；Baicalin；Cinnamates；HPLC；Content determination

[1]
咽炎片是由玄参、款冬花（制）、牡丹皮、木蝴蝶、地 性咽炎引起的咽干、咽痒、刺激性咳嗽等 。该制剂配伍
黄等12味药材组方而成的口服片剂，具有养阴润肺、清 药材中，玄参清热凉血、滋阴降火，为主药；牡丹皮清热
热解毒、清咽利喉、镇咳止痒等作用，临床上用于治疗慢 凉血，木蝴蝶清热利咽，款冬花润肺下气、止咳化痰，共
为臣药。已有研究分别对咽炎片中芍药苷、黄芩苷、芦
Δ 基金项目：山东省食品药品监督管理局 2018 年药品质量安全
丁、木蝴蝶苷 B 等成分进行含量测定 [2-5] ，但由于多种成
风险监测工作项目
分同时测定所需的对照品较多，而部分对照品价格高
＊主管中药师，硕士。研究方向：中药检验及质量标准。E-mail：
machh1111@126.com 昂，导致检验成本较高。一测多评法（Quantitative analy-

·2232 · China Pharmacy 2019 Vol. 30 No. 16 中国药房 2019年第30卷第16期