Safety Monitoring

Research on the detection method of Draconis Sanguis adulterated Resina Draconis in Zhenghonghua oil*

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  • Fujian Institute for Food and Drug Quality Control, Fuzhou 350012, China

Received date: 2023-06-19

  Online published: 2024-06-20

Abstract

Objective: To establish a screening method for the detection of adulteration of Draconis Sanguis in Zhenghonghua oil. Methods: To establish a thin layer chromatography (TLC) method with 7,4’-dihydroxyflavone as an index for fast screen of the adulteration in Zhenghonghua oil. The suspected samples were screened by TLC and the quantification was performed by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The chromatographic column was SuperLu C18 (2)(100 mm×2.1 mm,1.8 μm), the mobile phase was acetonitrile-water (25∶75) at a flow rate of 0.3 mL·min-1 and the column temperature was 25 ℃. The detection ion pairs for 7,4’-dihydroxyflavone were m/z 253.1→117.1 (quantitative) and m/z 253.1→91.0 (qualitative). Results: TLC method was specific and durable. The linear range of 7,4’-dihydroxyflavone was 0.470-37.58 ng·mL-1 (r=0.999 7) by UPLC-MS/MS. The average recovery rate(n=6) was 96.1% and RSD was 3.2%. Thirty batches of Zhenghonghua oil were screened by TLC, and 24 batches were suspected to have 7, 4’-dihydroxyflavone. The suspected samples were verified by UPLC-MS/MS, 24 batches of Zhenghonghua oil exceeded the proposed limit, and the verification results were consistent with TLC method. Conclusion:This method is rapid, accurate and can be used for the screening and analysis of adulterated Zhenghonghua oil.

Cite this article

LIU Yan-ting, CHEN Zai-min, WANG Yong . Research on the detection method of Draconis Sanguis adulterated Resina Draconis in Zhenghonghua oil*[J]. Chinese Journal of Pharmaceutical Analysis, 2024 , 44(4) : 620 -627 . DOI: 10.16155/j.0254-1793.2024.04.09

References

[1] 中华人民共和国药典2020年版. 一部[S]. 2020: 149
ChP 2020. Vol Ⅰ[S]. 2020: 149
[2] 赵江红. 高效液相色谱法鉴定29批血竭中非法添加的3种化学成分[J]. 中医研究, 2011, 24(8):17
ZHAO JH. Identification of three chemical components illegally added in 29 batches of Draconis Sanguis by high performance liquid chromatography[J]. Tradit Chin Med Res, 2011, 24(8):17
[3] 冼小敏, 林蔚文, 陈伟康, 等. HPLC-DAD法测定血竭饮片中添加苏丹红Ⅰ、Ⅱ、Ⅲ、Ⅳ及808猩红[J]. 药物分析杂志, 2020, 40(5):865
XIAN XM, LIN WW, CHEN WK, et al. Determination of Sudan scarlet added in Draconis Sanguis by HPLC-DAD[J]. Chin J Pharm Anal, 2020, 40(5):865
[4] 廖嘉宝, 张鹏, 谭沛, 等. 利用红外光谱法快速测定血竭中掺假松香的含量[J]. 浙江中医杂志, 2019, 54(9):695
LIAO JB, ZHANG P, TAN P, et al. The content of adulterated rosin in Draconis Sanguis was rapidly determined by infrared spectroscopy[J]. Zhejiang J Tradit Chin Med, 2019, 54(9):695
[5] 张明童, 刘志荣, 李冬华, 等. 薄层色谱法和高效液相色谱法鉴别掺伪龙血竭的血竭[J]. 理化检验-化学分册, 2020, 56(12):1267
ZHANG MT, LIU ZR, LI DH, et al. Identification of Draconis Sanguis adulterated with Resina Draconis by thin layer chromatography and HPLC[J]. Phys Test Chem Anal Part B: Chem Anal, 2020, 56(12):1267
[6] 薛恒跃, 邹亮, 秦峥. 含血竭中成药中掺杂龙血竭的鉴别研究[J]. 世界最新医学信息文摘, 2019, 19(66):36
XUE HY, ZOU L, QIN Z. Identification study of Resina Draconis mixed into traditional Chinese medicine containing Draconis Sanguis[J]. World Latest Med Inf, 2019, 19(66):36
[7] 张丽, 王绪平, 黄孝闻, 等. 血竭及龙血竭化学成分、药理作用研究进展[J]. 中国现代应用药学, 2019, 36(20):2605
ZHANG L, WANG XP, HUANG XW, et al. Advance of the chemical components and pharmacological effects of Draconis Sanguis and Resina Draconis[J]. Chin J Mod Appl Pharm, 2019, 36(20):2605
[8] 林忆龙, 文亦磊, 黄洪, 等. 龙血竭化学成分及药理作用研究进展[J]. 中国民族民间医药, 2020, 29(6):50
LIN YL, WEN YL, HUANG H, et al. Chemical constituents and pharmacological research of the Resina Draconis[J]. Chin J Ethnomed Ethnopharm, 2020, 29(6):50
[9] 屠鹏飞, 陶晶, 胡迎庆, 等. 龙血竭黄酮类成分研究[J]. 中国天然药物, 2003, 1(1):27
TU PF, TAO J, HU YQ, et al. Flavones from wood Dracaena conchinensis[J]. Chin J Nat Med,2003, 1(1):27
[10] 李云, 萧伟, 秦建平, 等. HPLC测定龙血竭提取物中龙血素A,B和7,4’-二羟基黄酮的含量[J]. 中国实验方剂学杂志, 2012, 18(3):45
LI Y, XIAO W, QIN JP, et al. Determination of loureirin A, B and 7, 4’-dihydroxy flavone in extract of Resina Draconis by HPLC[J]. Chin J Exp Tradit Med, 2012, 18(3):45
[11] 江立, 孙成逊, 田雪丽, 等. 龙血竭片中3种成分体外溶出度的测定[J]. 中成药, 2022, 44(4):1058
JIANG L, SUN CX, TIAN XL, et al. Determination of in vitro dissolution rates of three constituents in Longxuejie tablets[J]. Chin Tradit Pat Med, 2022, 44(4):1058
[12] 秦建平, 吴建雄, 李艳静, 等. DART/Q-TOF-MS快速鉴定龙血竭中5个酚酸类成分[J]. 药物分析杂志, 2014, 34(5):819
QIN JP, WU JX, LI YJ, et al. Rapid identification and characterization of five phenolic compounds in Resina Draconis by DART/Q-TOF-MS[J]. Chin J Pharm Anal, 2014, 34(5):819
[13] 李云, 萧伟, 秦建平, 等. HPLC同时测定龙血竭及其提取物中5个有效成分的含量[J]. 中国中药杂志, 2012, 37(7):929
LI Y, XIAO W, QIN JP, et al. Simultaneous determination of five active components in Resina Draconis and its extract by HPLC[J]. China J Chin Mater Med, 2012, 37(7):929
[14] 秦建平, 吴建雄, 李家春, 等. 不同产地龙血竭中5种成分的HPLC法测定[J]. 现代药物与临床, 2013, 28(4):547
QIN JP, WU JX, LI JC, et al. Determination of five components in Draconis Resina from different habitats by HPLC[J]. Drugs Clin, 2013, 28(4):547
[15] 万青, 王文清, 方建国, 等. 一测多评法测定龙血竭中5种有效成分[J]. 中草药, 2017, 48(21):4541
WAN Q, WANG WQ, FANG JG, et al. Determination of five active components in Draconis Resina by QAMS method[J]. Chin Tradit Herb Drugs, 2017, 48(21):4541
[16] 高柳, 张晓莉, 杨晨, 等. 超声波协同半仿生法提取龙血竭中4种成分的工艺研究[J]. 中国药师, 2021, 24(3):599
GAO L, ZHANG XL, YANG C, et al. Study on the ultrasonic-assisted semi-bionic extraction technology for 4 components from Resina Draconis[J]. China Pharm, 2021, 24(3):599
[17] 林爽, 王杰, 高珊珊, 等. 基于薄层色谱法和超高效液相色谱法对龙血竭的质量评价研究[J]. 中医药导报, 2023, 29(1):39
LIN S, WANG J, GAO SS, et al. Study on the quality evaluation of Longxuejie (Resina Draconis) based on TLC and UPLC[J]. Guid J Tradit Chin Med Pharm, 2023, 29(1):39
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