目的 选择合适的液相条件,建立加校正因子的主成分对照品外标法测定双氢青蒿素(DHA)中杂质DKA的方法。方法 采用C18色谱柱(4.6 mm×250 mm,5 μm);以乙腈-水(37∶63)为流动相,等度洗脱;流速为1 mL·min-1;检测波长为216 nm;柱温为15 ℃;进样体积为20 μL。结果 DHA α峰与其杂质DKA分离度良好,3根不同色谱柱测定出校正因子均值为0.256。结论 本方法测定DHA中杂质DKA准确、可靠,加校正因子的主成分对照品外标法可用于DHA原料药中DKA的质量控制。
Abstract
OBJECTIVE To establish a principal component reference substances external standard method with correction factor for the determination of impurity diketoal dehyde (DKA) in diketo aldehyde(DHA) bulk drug by selecting suitable liquid phase conditions. METHODS The chromatographic C18 column (4.6 mm×250 mm, 5 μm) was used; isometric elution was set at conducted using acetonitrile-water (37∶63) as elution condition; the flow rate was 1 mL·min-1; the detection wavelength was 216 nm; the column temperature was maintained at 15 ℃; the injection volume was 20 μL. RESULTS The DHA α peak and its impurity DKA were well separated. The average correction factor was 0.256 determined by three different chromatographic columns. CONCLUSION The correction factor of DKA in DHA is accurate and reliable. This method can be used for the quality control of DKA in DHA raw materials.
关键词
双氢青蒿素 /
diketo aldehyde /
校正因子
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Key words
dihydroartemisinin /
diketo aldehyde /
correction factor
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中图分类号：
R917
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参考文献
[1] TU Y Y. Artemisia Annua and Artemisinin Drugs(青蒿及青蒿素类药物)[M]. Beijing: Chemical Industry Press, 2015: 118.
[2] TJITRA E, HASUGIAN A R, SISWANTORO H, et al. Efficacy and safety of artemisinin-naphthoquine versus dihydroartemisinin-piperaquine in adult patients with uncompli-cated malaria: a multi-centre study in Indonesia. Malar J, 2012, 11(1):153-167.
[3] GRANDESSO F, GUINDO O, MESSE L W, et al. Efficacy of artesunateamodiaquine, dihydroartemisinin-piperaquine and artemetherlumefantrine for the treatment of uncom-plicated plasmodium falciparum malaria in Maradi, Niger. Malar J, 2018, 17(1): 52-61.
[4] LU Z H, PENG J H, ZHANG R X, et al. Dihydroartemisinin inhibits colon cancer cell viability by inducing apoptosis through up-regulation of PPARI expression. Saudi J Biol Sci, 2018, 25(2):372-376.
[5] LI Y W, ZHANG W, XU N, et al. Dihydroartemisinin inhibits the proliferation of pancreatic cancer JF-305 cells by regulating the expression of apoptosis-related proteins and the production of reactive oxygen species . China J Chin Mater Med(中国中药杂志), 2017, 42 (15):3026-3030.
[6] SHENG Q S, WANG W, GUO H W. Therapeutic effect and mechanism of dihydroartemisinin on primary liver cancer rats . Chin J Exp Tradit Med Form(中国实验方剂学杂志), 2014, 20 (14):150-154.
[7] CHENG Z, QI R, LI L, et al. Dihydroartemisinin ameliorates sepsis-induced hyperpermeability of glomerular endothelium via up-regulation of occludin expression. Biomed Pharmacother, 2018, 9:313-318.
[8] YE B, CHEN Y T, LIU C W. Effects of dihydroartemisinin on the ultrastructure of Pneumocystis carinii . Chin J Zoohoses(中国人兽共患病学报), 2000, 16 (4):21-24.
[9] DONG Y J, LI W D, TU Y Y, et al. Effects of dihydroartemisinin on autoantibody production, TNFalpha secretion and pathological changes of lupus nephritis in BXSB lupus mice . Chin J Integr Tradit West Med(中国中西医结合杂志), 2003, 23 (9):676-679.
[10] XU L M, CHEN X R. Effects of dihydroartemisinin on lupus BXSB mice . Chin J Dermatovenereol Inter Tradit West Med(中国中西医结合皮肤性病学杂志), 2002, 1(1):19-20.
[11] Ch.P(2015). Vol Ⅱ(中国药典2015年版.二部)[S]. 2015: 93.
[12] WANG K, ZHANG D, SUN P, et al. Determination of impurity diketo aldehyde in raw materials and tablets of dihydroartemisinin . China J Chin Mater Med(中国中药杂志), 2018, 43 (20):4069-4073.
[13] LIANG J. Evaluation and optimization of METHODS for determination of related substances of dihydroartemisinin in Chinese Pharmacopoeia 2015 edition . Sci Technol Eng (科学技术与工程), 2018,(15):220-226.
[14] LIANG J, ZHOU L, LUO L J, et al. Study on the transformation and determination of dihydroartemisinin epimer . Chin Pharm J(中国药学杂志), 2016, 51 (5):396-399.
[15] CABRI W, CIOGLI A, ILARIA D, et al. On-column epimerization of dihydroartemisinin: an effective analytical approach to overcome the shortcomings of the International Pharmacopoeia monograph. J Chromatogr B Analyt Technol Biomed Life Sci, 2008, 875(1):180-191.
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脚注
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基金
国家重大新药创制科技重大专项课题资助(2017ZX09101002-002);中国中医科学院院自主选题资助(zz10-002)
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