目的 采用HPLC-DAD/ELSD-ESI-TOF/MS对金鸣片中化学成分进行分析鉴别,建立其HPLC多指标定量指纹图谱,并为其质量控制提供科学依据。方法 采用Agilent SB C18柱(4.6 mm×250 mm,5 μm),以乙腈-0.2%乙酸水溶液为流动相,对金鸣片甲醇水提物进行梯度洗脱;柱温为25 ℃,体积流量为0.8 mL·min-1,进样量为30 μL,检测波长为280 nm。采用ESI-TOF/MS正、负离子模式扫描对其化学成分定性分析。结果 应用HPLC-DAD-ESI-TOF/MS从金鸣片中初步鉴别了20种化学成分,对其中5种主要成分进行了含量测定;在对多批次样品分析的基础上,建立了金鸣片多指标定量指纹图谱,结合相似度分析实现了对金鸣片的质量评价。结论 建立了金鸣片的化学成分分析和质量评价方法,为提高其质量评价标准提供了方法和技术支持。
Abstract
OBJECTIVE To analyze and identify the compositions using HPLC-DAD/ELSD-ESI-TOF/MS for establishing the multi index quantatitive HPLC fingerprint of the Jinming Tablet, in order to providing scientific basis for its quality control.METHODS The Agilent SB C18 column (4.6 mm×250 mm, 5 μm) was used with a mobile phase of acetonitrile-0.2% acetic acid in gradient elution, the flow rate was 0.8 mL·min-1, the sample voume was 30 μL, the column temperature was maintaine at 25 ℃, the detection wavelength was set at 280 nm. ESI-TOF/MS positive and negative ion mode scanning was used to qualitatively analyze the components in methanol water extract from Jinming Tablet.RESULTS Twenty compounds in Jinming Tablet extract could be primarily identified by HPLC-DAD on-line detection, in which five compounds were determined; based on the analysis of multiple batches of samples, the multi index chromatographic fingerprint was established, meanwhile combined with similarity analysis to achieve the quality evaluation of Jinming Tablet.CONCLUSION The HPLC-DAD/ELSD fingerprint film analysis method for Jinming Tablet is established, which could provide reference for the quality control of the material basis of other compound.
关键词
金鸣片 /
HPLC-DAD/ELSD-ESI-TOF/MS /
指纹图谱 /
多指标定量
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Key words
Jinming Tablet /
HPLC-DAD/ELSD-ESI-TOF/MS /
fingerprint /
multi index quantitation
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中图分类号：
R284
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参考文献
[1] CHEN Y C, XU S Q. Clinical observation on 40 cases of acute pharyngitis treated with Jin Ming Pian[J]. J Guiyang College of Tradit Chin Med(贵阳中医学院学报),1995,17(2):29-29.
[2] SHAO L, ZHUO L. A pharmaceutical study of Jin Ming Tablet[J]. Qilu Pharm Aff(齐鲁药事),1999,18(5):4-5.
[3] ZHENG Y Q, QU J Q, NIE H H, et al. Toxicological study of Jin Ming Tablet[J]. J Taishan Med College (泰山医学院学报),1989,10(Suppl 1):140-145.
[4] ZHAO H Q, DONG S S, CUI Q H, et al. Identification of active components in Syngnathus acus by HILIC-ESI-TOF/MS and study on their HILIC specific chromatograms[J]. Chin Tradit Herb Drugs(中草药), 2013, 44(13):1836-1841.
[5] LI G S, WANG H S. Determination of rehmannioside D in root of Rehmanniaglutinosa by HPLC[J].Chin Tradit Herb Drugs(中草药), 2003, 34(8):752-754.
[6] BAI Y E, YUAN P F, WANG Q H, et al. Determination of the content of crude drug and figwort Kazakhstan Pakistan glycoside and harpagoside HPLC-UV wavelength conversion method[J]. China J Chin Mater Med (中国中药杂志), 2011,46(19):2697-2702.
[7] LAN T F, WANG X, WANG D J, et al. Determination of four tanshinones in Salviae Miltiorrhizae Radix et Rhizoma with quantitative analysis of multi-components by single-marker[J].Chin Tradit Herb Drugs(中草药), 2012, 43(12):2420-2423.
[8] CAO J J, LIANG Z S, YANG D F, et al. Establishment of HPLC-DAD multi-wavelength chromatographic fingerprints of Rehmanniae Radix and its application in processing Rehmanniae Radix Praeparae[J]. Chin Tradit Herb Drugs(中草药), 2014, 45(2):265-270.
[9] LIU Y F, LIANG D, LUO H, et al. Chemical constituents from root tubers of Rehmannia glutinosa[J]. Chin Tradit Herb Drugs(中草药), 2014, 45(1):16-22.
[10] WANG J Z, LIU Z, MA L M, et al. Identification of chemical constituents in Scrophulariae Radix by HPLC-IT-TOF-MS[J]. China J Chin Mater Med(中国中药杂志), 2016, 41(7):1257-1268.
[11] SAHO Y L, CAO G.Rapid determination of tanshinone Ⅱ A in Radix Salviae Miltiorrhizae by near-infrared spectroscopy coupled with liquid chromatography[J]. Chin Med Rep(中国医药导报), 2014, 11(9):135-137.
[12] YUAN C L, SUN L, YUAN S T, et al. Pharmacological activities and possible mechanism of effective components in Ophiopogonis Radix[J]. Chin J New Drugs(中国新药杂志), 2013,22(21):2496-2502.
[13] GUO R, CHEN Y C, LI X H, et al. Determination of 6 kinds of indexes in Niuhuang Jiedu Tablets[J]. J Shenyang Pharm Univ(沈阳药科大学学报), 2016, 33(6):454-457.
[14] XIE X Y, XIA C S. Advances in studies on chemical constituents and pharmacological activities of Scrophularia ningpoensis Hemsl[J]. Asia-Pacific Tradit Med(亚太传统医药), 2010, 6(5):121-125.
[15] ZHU Y L. Content determination of ruscogenin in Shengmaiyin by HPLC-ELSD[J]. Heilongjiang Med J(黑龙江医药), 2014(6):1281-1283.
[16] WEI C R.Research advance in pharmacological effect of borneol and the underlying mechanism[J]. Inter J Pathol Clin Med(临床与病理杂志), 2010, 30(5):447-451.
[17] SUN X P, OU L J, MI H Q, et al. A nalgesic and anti-inflammation effect of borneol[J]. Tradit Chin Drug Res Clin Pharm(中药新药与临床药理), 2007, 18(5):353-355.
[18] WEN Y J, SHEN X L, WANG Y J.Process for preparing high-purity borneol by borneol[J]. Chin Tradit Pat Med(中成药), 2016, 38(1):215-218.
[19] HONG C J, RAO H M.Determination of borax in Ding Ding cream by high performance liquid chromatography[J]. Strait Pharm J(海峡药学), 2010, 22(7):105-107.
[20] PANG Y P, ZHAO Z P, WU G C, et al.Determination of borax in flour products by high performance liquid chromatography[J]. Food Ferment Ind(食品与发酵工业), 2009,35(8):126-128.
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脚注
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基金
山东省自然科学基金项目资助(ZR2017LH069, ZR2017LH071);山东省科技发展计划项目资助(2016GSF202011,2016GSF202014);山东省泰山学者岗位资助(郭兰萍);山东省科学院先导专项资助(郭兰萍)
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