GC法测定马香苓口服液中百秋李醇含量研究

doi:10.16431/j.cnki.1671-7236.2020.07.033

中国畜牧兽医 ›› 2020, Vol. 47 ›› Issue (7): 2264-2276.doi: 10.16431/j.cnki.1671-7236.2020.07.033

GC法测定马香苓口服液中百秋李醇含量研究

杨洪早^1,4, 李锦宇¹, 王东升¹, 张世栋¹, 董书伟¹, 闫宝琪¹, 那立冬^1,4, 吴春丽³, 邓俊³, 吴冠连³, 陈新丽³, 赵留涛³, 朱凯³, 梁永喜³, 严作廷^1,2

1. 中国农业科学院兰州畜牧与兽药研究所, 兰州 730050;
2. 农业农村部兽用药物创制重点实验室, 兰州 730050;
3. 郑州大学药学院, 郑州 450001;
4. 甘肃农业大学动物医学院, 兰州 730070

收稿日期:2019-12-17 出版日期:2020-07-20 发布日期:2020-07-18
通讯作者: 王东升(1979-),男,甘肃临洮人,副研究员,研究方向:中药药理与奶牛繁殖疾病,E-mail:lzmyswdsh@126.com;严作廷(1962-),男,甘肃武威人,博士,研究员,博士生导师,研究方向:中兽药研发,奶牛疾病诊断和预防,E-mail:yanzuoting@caas.cn E-mail:lzmyswdsh@126.com;yanzuoting@caas.cn
作者简介:杨洪早(1992-),男,云南临沧人,硕士生,研究方向:中兽药研究与开发,E-mail:yhz03008@163.com
基金资助:
"十三五"国家重点研发计划项目（2017YFD0502201）；中国农业科学院农业科技创新工程（CAAS-ASTIP-2017-LIHPS-03）；甘肃省科技支撑计划项目（1504NKCA052）

Determination of Patchouli Alcohol in Maxiangling Oral Liquid by GC

YANG Hongzao^1,4, LI Jingyu¹, WANG Dongsheng¹, ZHANG Shidong¹, DONG Shuwei¹, YAN Baoqi¹, NA Lidong^1,4, WU Chunli³, DENG Jun³, WU Guanlian³, CHEN Xinli³, ZHAO Liutao³, ZHU Kai³, LIANG Yongxi³, YAN Zuoting^1,2

1. Lanzhou Institute of Animal Husbandry and Pharmaceutical Sciences, Chinese Academy of Agricultural Sciences, Lanzhou 730050, China;
2. Key Laboratory of Veterinary Pharmaceutical Discovery, Ministry of Agriculture and Rural Affairs, Lanzhou 730050, China;
3. College of Pharmacy, Zhengzhou University, Zhengzhou 450001, China;
4. College of Veterinary Medicine, Gansu Agricultural University, Lanzhou 730070, China

Received:2019-12-17 Online:2020-07-20 Published:2020-07-18

摘要/Abstract

摘要： 试验旨在建立测定马香苓口服液中百秋李醇含量的研究方法。本研究采用气相色谱法，其色谱条件是使用色谱柱HP-5毛细管柱；柱温采用程序升温（初始温度150 ℃，保持18 min，以50 ℃/min速率升至280 ℃，保持5 min）；进样口温度为280 ℃；载气：高纯氮气；流速1 mL/min；进样量1 μL，分流比20：1；检测器为氢火焰离子化检测器，温度为280 ℃；氢气流速40 mL/min，空气流速370 mL/min；分别进行系统适用性试验、专属性试验、线性范围考察、检测限和定量限的确定、精密度试验、稳定性试验、重复性试验、加样回收率试验、耐用性试验，并对10批样品进行了含量测定。结果显示，专属性溶液中的溶剂峰、药液的杂质峰与主成分峰能达到有效分离且分离度符合要求（R ≥ 1.5），表明该方法系统适用性良好；阴性对照溶液未检出色谱峰，表明样品中其他成分不干扰测定；百秋李醇定量限和检测限分别为2.842和0.812 μg/mL；百秋李醇检测质量浓度在15.86~1 015 μg/mL范围内与峰面积积分值呈良好的线性关系（y=0.869x-10.45，R²=0.999，n=7）。精密度试验、稳定性试验（日内和日间精密度）、重复性试验的平均RSD分别为0.90%、1.63%和1.83%、2.90%，其RSD均在可控范围内（RSD ≤ 3%）；平均加样回收率为95.36%，RSD=2.82%（n=6），表明所建立的气相色谱法检测百秋李醇的含量回收率良好；进行耐用性试验，最终验证所建立的色谱方法可以稳定检测百秋李醇的含量。经方法学验证，该方法准确稳定，简便可行，能够作为马香苓口服液君药广藿香中百秋李醇的含量控制方法，同时也为该制剂质量控制提供了一种有效的检测方法，暂定本品中广藿香药材按百秋李醇计不少于47.53 μg/mL。

关键词: 马香苓口服液; 气相色谱法; 广藿香; 百秋李醇; 含量测定

Abstract: The purpose of the experiment was to establish a capillary gas chromatography (GC) method for the content determination of patchouli alcohol in Maxiangling oral liquid.The samples were determined by capillary GC.The chromatographic conditions were as follows:The chromatographic column HP-5 capillary column was used,and the column temperature was controlled by programming (the initial temperature was 150 ℃,held for 18 min,and then rose at a rate of 50 ℃/min up to 280 ℃ for 5 min).The injector temperature was 280 ℃.Carrier gas was high purity nitrogen.The flow rate was 1 mL/min.The injection volume was 1 μL,and the split ratio was 20:1.FID detector was used and the detector temperature was 280 ℃.Hydrogen flow rate was 40 mL/min and air flow rate was 370 mL/min.The system applicability test,specificity test,linear range test,determination of detection limit and quantitative limit,precision test,stability test,repeatability test,sample recovery test,durability test and content determination of ten batches of samples were conducted.The results showed that the solvent peak,impurity peak and main component peak in the specific solution could be separated effectively and the resolution of the chromatographic method met the requirements (R ≥ 1.5),which showed that the method had good applicability.No outstanding peak was detected in the negative control solution,indicating that other components in the sample did not interfere with the determination.Limit of quantitation(LOQ) and limit of detection(LOD) of patchouli alcohol were 2.842 and 0.812 μg/mL.Under the above chromatographic conditions,a good linearity was obtained in the range of 15.86-1 015 μg/mL (y=0.869x-10.45,R²=0.999,n=7);RSDs of precision,stability(intra-day precision and daytime precision) and reproducibility tests were 0.90%,1.63%and 1.83%,2.90%,respectively.RSDs were within controllable range (RSD ≤ 3%).The average recovery was 95.36%,with a RSD of 2.82%(n=6).The results showed that the established gas chromatography method had a good recovery rate for the determination of patchouli alcohol.The durability test was carried out to verify that the established chromatographic method could stably determine the content of patchouli alcohol.The methodological verification showed that the GC method was accurate,stable,convenient and feasible,and could be used as a method for the content control of patchouli alcohol in Maxiangling oral liquid.At the same time,it also provided an effective detection method for the quality control of this preparation.It was tentatively determined that the content of patchouli alcohol in this product was not less than 47.53 μg/mL.

Key words: Maxiangling oral liquid; GC; Pogostemon cablin; patchouli alcohol; content determination

中图分类号:

S859.3

杨洪早, 李锦宇, 王东升, 张世栋, 董书伟, 闫宝琪, 那立冬, 吴春丽, 邓俊, 吴冠连, 陈新丽, 赵留涛, 朱凯, 梁永喜, 严作廷. GC法测定马香苓口服液中百秋李醇含量研究[J]. 中国畜牧兽医, 2020, 47(7): 2264-2276.

YANG Hongzao, LI Jingyu, WANG Dongsheng, ZHANG Shidong, DONG Shuwei, YAN Baoqi, NA Lidong, WU Chunli, DENG Jun, WU Guanlian, CHEN Xinli, ZHAO Liutao, ZHU Kai, LIANG Yongxi, YAN Zuoting. Determination of Patchouli Alcohol in Maxiangling Oral Liquid by GC[J]. China Animal Husbandry and Veterinary Medicine, 2020, 47(7): 2264-2276.

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GC法测定马香苓口服液中百秋李醇含量研究

Determination of Patchouli Alcohol in Maxiangling Oral Liquid by GC

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