中国药物警戒 ›› 2024, Vol. 21 ›› Issue (3): 295-299.
DOI: 10.19803/j.1672-8629.20230521

• 药品质量控制及评价专栏 • 上一篇    下一篇

顶空-气相色谱法测定到手香提取物11种溶剂残留量

王丹丹, 王莹Δ, 姚令文, 刘芫汐, 金红宇#, 马双成*   

  1. 中国食品药品检定研究院中药民族药检定所,北京102600
  • 收稿日期:2023-08-23 出版日期:2024-03-15 发布日期:2024-03-18
  • 通讯作者: *马双成,男,研究员·博导,中药民族药物质基础与质量安全评价研究。E-mail: msc@nifdc.org.cn;#为共同通信作者。
  • 作者简介:王丹丹,女,本科,药物分析。Δ为并列第一作者。
  • 基金资助:
    国家重点研发计划（2022YFC3501505）

Determination of residual solvents in extract of Coleus amboinicus by headspace-gas chromatography

WANG Dandan, WANG YingΔ, YAO Lingwen, LIU Yuanxi, JIN Hongyu#, MA Shuangcheng*   

  1. Institute for Control of Chinese Traditional Medicine and Ethnic Medicine, National Institutes for Food and Drug Control, Beijing 102600, China
  • Received:2023-08-23 Online:2024-03-15 Published:2024-03-18

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摘要： 目的 建立顶空-气相色谱法测定中药到手香提取物中苯、丙烯腈、甲基丙烯酸甲酯、甲苯、1,2-二氯乙烷、对二甲苯、间二甲苯、邻二甲苯、氯苯、苯乙烯和二乙烯苯11种溶剂残留的分析方法。方法 供试品经顶空进样器85℃平衡45 min,分流比10∶1（V∶V）,采用DB-WAX聚乙二醇为固定相的弹性石英毛细管柱（长30 m,内径0.32 mm,膜厚0.5 μm）,FID氢火焰离子化检测器进行分析。结果 11种挥发性有机物分离效果较好,在0.22~23.86 μg·mL-1的浓度范围内线性关系良好（r≥0.99）;方法定量限为0.008 4 μg·mL-1≤LOQ≤0.543 2 μg·mL-1;低、中、高水平下各成分的平均回收率为84%~103%之间;相对标准偏差≤10 %（n=6）,经方法学验证后该方法符合实验要求。3批样品中甲苯、间二甲苯、邻二甲苯及二乙烯基苯有检出,低于定量限,均未超标。结论 该方法易于操作,结果可靠,可用于中药到手香提取物中的残留溶剂检测,亦为其他中药提取物中残留溶剂分析提供方法参考,确保用药安全。

关键词: 到手香, 提取物, 挥发性化合物, 溶剂残留, 顶空-气相色谱法, 大孔树脂, 质量控制, 药物警戒

Abstract: Objective To establish a headspace-gas chromatography method for the determination of residues of benzene, acrylonitrile, methyl methacrylate, toluene, 1, 2-dichloroethane, p-xylene, m-xylene, o-xylene, chlorobenzene, styrene and divinylbenzene in Coleus amboinicus extracts, which is a traditional Chinese medicine (TCM). Methods The samples were balanced by a headspace injector at 85℃ for 45 min, and the split ratio was 10:1 (V : V). The DB-WAX capillary column (30 m long, 0.32 mm wide, and 0.5 μm thick), which was fixed using polyethylene glycol, was used to separate samples, while a flame ionization detector (FID) was used for analysis. Results The eleven volatile organic compounds were well-separated. Experimental results showed that the linearity of these volatile organic compounds ranged from 0.22 μg·mL-1 to 23.86 μg·mL-1 with correction coefficients above 0. 99. The limit of quantification was between 0.008 4 μg·mL-1 and 0.543 2 μg·mL-1. The average recovery of the target compounds ranged from 84% to 103% at three spike levels, with relative standard deviations less than 10.0% (n=6), which met the requirements of trace determination. Toluene, m-xylene, o-xylene and divinylbenzene were detected in three batches of samples, but below the limit of quantitation and the standard. Conclusion This method is simple, reliable, and applicable to the detection of residual solvents in the extract of Coleus amboinicus, which can facilitate the analysis of residual solvents in other TCM extracts and medication safety.

Key words: Coleus amboinicus, extracts, volatile organic compounds, solvent residues, headspace-gas chromatograph, macroporous resin, quality control, pharmacovigilance

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