Biological Fingerprinting Analysis of Interaction Between Taxoids in Taxus and Microtubule Protein by Microdialysis Coupled with High-performance Liquid Chromatography/Mass Spectrometry for Screening Antimicrotubule Agents

Some natural products, such as traditional Chinese medicines（TCMs）, contain compounds with anticancer activity and have attracted a great interest in recent years as alternative anticancer therapies. A quick and convenient assay for screening antimicrotubule compounds in which in vitro microdialysis/high-performance liquid chromatography （HPLC） is used to monitor the binding of the compounds extracted from TCM Taxus cuspidata Siebold ＆ Zucc（Taxus） to microtubules is reported. It was observed that the extract of Taxus contains at least five compounds which have affinity interaction with microtubules by biological fingerprinting analysis, and they were identified as the taxoids of taxol, baccatin III, 10-deacetylbaccatin Ⅲ（10-DAB）, cephalomannine and 7-epi-10-deacetyltaxol （7-epi-10-DAT） based on the comparison of their high-performance liquid chromatographic/mass spectrometric and UV spectra with those of the standard samples, both assembly-promoting and disassembly-inhibiting characteristics of those compounds were evaluated. It was observed that baccatin Ⅲ and 10-DAB bound to microtubules and the binding degrees were influenced by GTP. Competitive binding behavior of taxol with other four taxoids to microtubules was also investigated.

Quantification of six bioactive compounds in Zhenqi Fuzheng preparation by high-performance liquid chromatography coupled with diode array detector and evaporative light scattering detector

A simple and accurate high-performance liquid chromatography（HPLC）coupled with diode array detector（DAD）and evaporative light scattering detector（ELSD）was established for the determination of six bioactive compounds in Zhenqi Fuzheng preparation（ZFP）.The monitoring wavelengths were 254,275 and 328 nm.Under the optimum conditions,good separation was achieved,and the assay was fully validated in respect of precision,repeatability and accuracy.The proposed method was successfully applied to quantify the six ingredients in 31 batches of ZFP samples and evaluate the variation by hierarchical cluster analysis（HCA）,which demonstrated significant variations on the content of these compounds in the samples from different manufacturers with different preparation procedures.The developed HPLC method can be used as a valid analytical method to evaluate the intrinsic quality of this preparation.

HPLC多指标成分定量、化学计量学及熵权-TOPSIS分析在龙葵综合质量评价中的应用

目的建立不同产地龙葵中11个成分含量同步检测方法,并采用化学计量学和熵权-TOPSIS法对其质量进行评价。方法收集8省17个批次龙葵样品,采用HPLC法同时检测龙葵中梣皮树脂醇、松脂素、槲皮素、芦丁、澳洲茄碱、澳洲茄边碱、客西茄碱、澳洲茄胺、去半乳糖替告皂苷、薯蓣皂苷元和β-谷甾醇的含量,建立龙葵多组分定量控制模式;采用化学识别模式和熵权-TOPSIS法建立龙葵质量优劣评价模型,对其整体质量进行综合评价。结果11个成分分别在0.78~39.00,0.55~27.50,0.34~17.00,0.21~10.50,41.87~2093.50,60.95~3047.50,2.58~129.00,1.02~51.00,0.46~23.00,1.05~52.50,0.42~21.00μg/mL(r>0.9990)范围内线性关系良好,平均加样回收率在96.81%~100.28%范围内(RSD<2.0%,n=9);17批样品聚为3类;澳洲茄边碱、澳洲茄碱、去半乳糖替告皂苷和梣皮树醇可能是影响龙葵产品质量主要潜在标志物;熵权-TOPSIS法分析结果显示17批龙葵质量评价贴近度分别为0.4336、0.4168、0.6242、0.5008、0.4791、0.6361、0.5683、0.2500、0.1909、0.2221、0.1707、0.7200、0.6983、0.7447、0.7179、0.7209、0.7183,辽宁、吉林和黑龙江产地龙葵整体质量较好,其次为江苏、河南和安徽产地。结论建立的同时测定龙葵中11种成分含量的HPLC法,操作便捷,结果准确;化学计量学及熵权-TOPSIS法客观全面,可用于龙葵的整体质量评价。

Comparative analysis of four edible mushrooms based on HPLC fingerprint and pattein recognition analysis

A high performance liquid chromatography-ultraviolet(HPLC-UV)fingerprint method for the overall chemical analysis of edible mushrooms was established based on Auricularia heimuer for the first time,and then applied to analyze 60 batches of A.heimuer,Auricularia cornea.Auricularia cornea*Yu Muer’and TremeUa fuciformis.A total of 9 characteristic peaks of A.heimuer.11 characteristic peaks of A.cornea,6 characteristic peaks of A.cornea‘Yu Muer’,and 9 characteristic peaks of I fuciformis were designated.Then,a combinatory analysis,including similarity evaluation,hierarchical cluster analysis and principal component analysis,revealed the chemical consistency and difference between samples from the same and different species.The HPLC fingerprint method established in this paper could be used to characterize the components of A.heimuer,A.cornea,A.cornea‘Yu Muer’,and T.fuciformis and discriminate the 4 edible mushrooms effectively in combination with pattern recognition analysis.

基于UPLC指纹图谱与抗氧化谱效关系的枸杞子质量标志物研究

目的:建立基于超高效液相色谱法(UPLC)指纹图谱与抗氧化谱效关系的枸杞子质量标志物研究方法,为其质量评价提供依据。方法:采用UPLC建立31批枸杞子指纹图谱,基于指纹图谱共有峰峰面积结果,采用聚类分析、主成分分析(PCA)、正交偏最小二乘法-判别分析(OPLS-DA)方法评价枸杞子整体质量并筛选出主要质量标志物。以多功能氧化酶(MFO)、1,1-二苯基-2-三硝基苯肼(DPPH)、总抗氧化能力(T-AOC)的测定值评价枸杞子的抗氧化能力,利用双变量相关性分析法与正交偏最小二乘法-回归分析研究指纹图谱共有峰与抗氧化活性指标的谱效关系,综合分析筛选质量标志物。结果:枸杞子UPLC指纹图谱共确定34个共有峰,31批枸杞子聚为3类,可区分不同产地的枸杞子;PCA得到4个影响枸杞子分类的主要因子;OPLS-DA显示共有峰2、7、17、19、33的化合物可作为鉴别和区分枸杞子的主要质量标志物;双变量相关性分析表明峰8、11、15、20、23、34的化合物与MFO、DPPH、T-AOC的测定值呈极显著相关,正交偏最小二乘法-回归分析表明峰11、15、23、25、31、33、34的化合物是主要的活性成分群,此类成分可作为枸杞子抗氧化活性的质量标志物。结论:研究结果阐明了枸杞子抗氧化活性的物质基础,筛选出的质量标志物可为枸杞子的质量控制与评价提供依据。

五味子配方颗粒UPLC指纹图谱研究及6个成分含量测定

目的:建立五味子配方颗粒UPLC指纹图谱,并对其所含的6个有效成分进行定量分析。方法:以超高效液相色谱法,采用色谱柱ACQUITY UPLC?HSS T3(2.1 mm×100 mm;1.8μm);流动相:乙腈-0.1%磷酸溶液梯度洗脱;流速:0.4 mL·min^(-1);检测波长:检测波长为260 nm(前17 min),后变换为215 nm进行分析。结果:五味子配方颗粒指纹图谱共标定14个共有峰,与对照指纹图谱相似度大于0.90。五味子醇甲、五味子醇乙、当归酰基戈米辛H、五味子酯乙、五味子甲素和五味子乙素在8.626~552.089μg·mL^(-1)(r=1.000)、2.489~159.27μg·mL^(-1)(r=1.000)、1.868~119.521μg·mL^(-1)(r=1.000)、1.032~66.062μg·mL^(-1)(r=1.000)、0.990~63.362μg·mL^(-1)(r=1.000)、1.199~76.753μg·mL^(-1)(r=1.000)范围内线性关系良好;平均加样回收率(RSD)分别为95.9%(1.7%)、95.7%(1.5%)、95.9%(1.8%)、94.9%(0.8%)、97.1%(3.8%)、94.2%(1.7%)(n=9)。结论:建立了五味子配方颗粒的指纹图谱及同时测定其6种主要成分含量的方法,操作简便,结果稳定、准确,对建立五味子配方颗粒的质量控制标准提供了依据,具有重要的应用价值。

Differentiation of Belamcandae Rhizoma and Iridis Tectori Rhizoma by Thin-Layer Chromatography and High-Performance Liquid Chromatography

Objective:Belamcandae Rhizoma and Iridis Tectori Rhizoma are easily confused with each other.The main objective of this study is to distinguish them using chemical analysis.Materials and Methods:Thin-layer chromatography(TLC)and high-performance liquid chromatography(HPLC)fingerprint methods were established to compare the chemical profile,while HPLC quantitation was used to determine the contents of three isoflavones in thirty batches of Belamcandae Rhizoma and Iridis Tectori Rhizoma samples.Results:The two herbs could be distinguished by TLC using acetic acid-n hexane-ethyl acetate(1:90:80 v/v/v)as the mobile phase,according to the fluorescent band under 366 nm at R_(f) 0.2.In total,12 compounds were identified in the 24-min HPLC fingerprint.The similarity coefficient between the two herbs was 0.54±0.01.Mangiferin(1),tectoridin(2),iridin(3),irigenin(5),irisflorentin(6),and iristectorin A(9)were the main peaks in Belamcandae Rhizoma,while tectoridin(2)and tectorigenin(4)were the major peaks in Iridis Tectori Rhizoma.The contents of 2 in Iridis Tectori Rhizoma(2.50±0.20%)were 8.93 times higher than that of Belamcandae Rhizoma(0.28±0.08%),while the ones of 5 and 6 were slightly lower in Iridis Tectori Rhizoma.Conclusions:The study established fast and effective methods to distinguish Belamcandae Rhizoma from Iridis Tectori Rhizoma.

Comprehensive Quality Evaluation of ShuXueNing Injection Employing Quantitative High-Performance Liquid Chromatography Fingerprint and Chemometrics

Objective:In this study,a comprehensive and effective quality method for evaluating the efficacy of ShuXueNing injection(SXNI)was developed.Materials and Methods:Quantitative high-performance liquid chromatography fingerprint,the quantitative analysis of multicomponents by a single marker(QAMS)method,hierarchical cluster analysis(HCA),and orthogonal partial least squares discrimination analysis(OPLS-DA)were used to distinguish 53 batches of SXNI samples from 7 manufacturers.Results:A total of 53 batches of samples were analyzed to establish antithesis fingerprint of SXNI,and 12 peaks of the common model were collected and used for the similarity analysis.Meanwhile,six index flavonoid components were determined by the QAMS method,using rutin as internal reference substance.The accuracy of the QAMS method was confirmed by investigating the relative deviation between the QAMS method and the traditional external standard method.The results demonstrated that there was no significant difference(RE<1%),suggesting that QAMS was a reliable and convenient method for the content determination of multiple components.The HCA and OPLS-DA methods drew a similar conclusion.The 53 batches of SXNI samples from 7 manufacturers were categorized into five groups,indicating that chemometrics could reveal the quality differences of SXNI between the manufacturers.Conclusions:The method established herein was efficient and successful in assessing the quality of SXNI,and that it may be potentially employed in the quality control of related products composed of Ginkgo biloba extract.

UPLC-MS/MS法同时测定同仁牛黄清心丸中15个胆汁酸的含量

目的 建立同时测定同仁牛黄清心丸中15个胆汁酸成分含量的方法,并采用该法测定15批样品的含量。方法 以脱氢胆酸为内标,采用超高效液相色谱-串联质谱(UPLC-MS/MS)技术进行测定。色谱柱为Hypersil GOLD C_(18),以甲醇-0.1%甲酸溶液为流动相进行梯度洗脱,流速为0.2 mL/min,柱温为40℃,进样量为2μL;采用加热型电喷雾离子源,在负离子模式下进行平行反应监测模式扫描。采用SPSS 24.0软件对含量测定结果进行化学模式识别分析。结果 15个胆汁酸成分在各自检测质量浓度范围内与峰面积线性关系良好(R^(2)均不小于0.998 9),精密度、重复性、稳定性均良好(RSD均不大于5.49%),平均加样回收率为93.8%~105.7%(RSD为0.5%~5.8%)。牛磺胆酸、7-酮-3α,12α-羟基胆烷酸、12-脱氢胆酸、甘氨胆酸、3-oxo-7α,12α-hydroxy-5β-cholanoic acid、牛磺鹅脱氧胆酸、3α-羟基-7-氧代-5β-胆烷酸、猪胆酸、牛磺脱氧胆酸钠、猪脱氧胆酸、胆酸、甘氨鹅脱氧胆酸、甘氨脱氧胆酸、鹅脱氧胆酸、脱氧胆酸的平均含量分别为670.56、25.97、10.54、280.12、4.04、29.81、182.98、813.55、120.95、220.31、797.37、18.37、68.59、30.13、59.82μg/g。聚类分析和主成分分析均将15批同仁牛黄清心丸分为2类,其中S1~S12为一类,S13~S15为另一类。结论 所建方法准确、灵敏度高、专属性强,且测定胆汁酸种类较多,能快速实现对同仁牛黄清心丸中15个胆汁酸成分的定量分析,适用于该药的质量控制。

隔山消的指纹图谱建立、化学模式识别分析及多指标含量测定

目的建立隔山消药材的指纹图谱并进行化学模式识别分析,同时测定其中4种成分的含量。方法采用高效液相色谱(HPLC)法。色谱柱为ACE UExcel C_(18),流动相为乙腈-0.1%磷酸溶液(梯度洗脱),流速为1.2 mL/min,检测波长为210 nm,柱温为40℃,进样量为10μL。以青阳参苷元为参照,采用《中药色谱指纹图谱相似度评价系统(2012版)》绘制16批隔山消药材的HPLC指纹图谱并进行相似度评价,确定共有峰。采用SPSS 26.0软件和SIMCA 14.0软件进行聚类分析、主成分分析和正交偏最小二乘-判别分析,以变量重要性投影(VIP)值大于1为标准筛选影响隔山消药材质量的差异性成分;采用相同的HPLC法测定丁香酸、去酰基萝藦苷元、白首乌二苯酮和青阳参苷元的含量。结果16批隔山消药材中共有29个共有峰,相似度为0.723~0.998;共指认了4个共有峰,分别为丁香酸(7号峰)、去酰基萝藦苷元(9号峰)、白首乌二苯酮(13号峰)、青阳参苷元(15号峰)。聚类分析结果显示,16批隔山消药材可聚为3类,其中S1为一类,S3为一类,S2、S4~S16为一类。主成分分析结果显示,5个主成分的累计方差贡献率为88.706%,分类结果与聚类分析结果一致。正交偏最小二乘-判别分析结果显示,VIP值大于1的共有峰由大到小依次为20号峰、10号峰、25号峰、12号峰、15号峰(青阳参苷元)、21号峰、14号峰、16号峰、26号峰、22号峰、17号峰。丁香酸、去酰基萝藦苷元、白首乌二苯酮和青阳参苷元检测质量浓度的线性范围分别为0.7153~45.7780、2.3794~152.2810、0.6420~41.0850、14.5416~930.6620μg/mL(R^(2)均大于0.999);定量限分别为0.3577、0.4759、0.6420、2.4236μg/mL,检测限分别为0.1460、0.1641、0.2488、0.8333μg/mL;精密度、重复性、稳定性(24 h)试验的RSD均小于3%;平均加样回收率分别为99.11%(RSD=2.00%,n=9)、98.54%(RSD=2.21%,n=9)、96.33%(RSD=2.54%,n=9)、95.96%(RSD=2.93%,n=9);含量分别为17.12~147.80、95.23~583.10(S8低于定量限)、16.91~210.88、211.68~3587.15(S1低于定量限)μg/g。结论所建HPLC指纹图谱和含量测定方法稳定、可靠、准确度高且重复性好,结合化学模式识别分析可用于隔山消药材的质量控制。

基于超高效液相色谱-高分辨质谱联用技术的桑黄干预后大鼠尿液代谢组学分析

为探讨服用桑黄水煎液对机体的影响,采用超高效液相色谱-高分辨质谱(UPLC-HDMS)联用技术,检测灌胃给予桑黄水煎液后大鼠尿液中代谢物的变化。采用正交偏最小二乘法判别分析(OPLS-DA)对空白组和给药组大鼠尿液代谢物进行聚类分析,筛选出潜在的生物标志物,并通过MetaboAnalyst 3.0网站分析相关代谢通路。数据显示,两组大鼠尿液中的代谢物在第28天得到了很好的区分,发现并鉴定了10个生物标记物。灌胃给予桑黄水煎液主要对机体的半胱氨酸和甲硫氨酸代谢、精氨酸和脯氨酸代谢、嘌呤代谢等代谢通路产生影响。研究结果为深入探讨桑黄药效作用机制奠定了一定的实验基础。

田基黄高效液相色谱指纹图谱共有模式的研究

高效液相色谱指纹图谱已经普遍应用于中药材及制剂的分析检测,在用高效液相色谱指纹图谱进行分析中,建立图谱的共有模式是关键的一环,共有模式的好坏直接影响分析的结果.以田基黄的高效液相色谱指纹图谱为例,说明了一种建立共有模式行之有效的方法.

蒲蓝利咽合剂的指纹图谱建立及含量测定

目的建立蒲蓝利咽合剂的指纹图谱和绿原酸等8种成分的含量测定方法,以评价蒲蓝利咽合剂的质量。方法以黄芩苷为参照峰,采用《中药色谱指纹图谱相似度评价系统(2012版)》建立11批蒲蓝利咽合剂的高效液相色谱(HPLC)指纹图谱,指认共有峰并进行相似度评价,采用SPSS 20.0、SIMCA 14.1软件进行聚类分析、主成分分析、正交偏最小二乘法-判别分析,以变量重要性投影(VIP)值大于1为指标筛选影响蒲蓝利咽合剂质量的标志物;采用相同的HPLC法测定绿原酸等8种成分的含量。结果11批蒲蓝利咽合剂指纹图谱共有20个共有峰,相似度在0.973~0.994之间;指认了8个共有峰,分别为绿原酸、咖啡酸、马钱苷、菊苣酸、木蝴蝶苷B、黄芩苷、千层纸素A-7-O-β-D-葡萄糖醛酸、汉黄芩苷。聚类分析结果显示,11批样品分为2大类,其中S3、S10~S11为一类,其余为一类。主成分分析结果显示,前4个主成分的累计方差贡献率为95.546%,其分类结果与聚类分析结果一致。正交偏最小二乘法-判别分析结果显示,15、14(黄芩苷)、10、18(汉黄芩苷)、11、17(千层纸素A-7-O-β-D-葡萄糖醛酸)、4、20、16、12、7、19号峰的VIP值大于1。11批样品中绿原酸、咖啡酸、马钱苷、菊苣酸、木蝴蝶苷B、黄芩苷、千层纸素A-7-O-β-D-葡萄糖醛酸、汉黄芩苷的含量分别为0.287~1.021、0.163~0.485、0.735~3.641、0.587~4.012、1.920~9.063、37.443~115.974、3.623~13.942、7.135~18.736 mg/g。结论建立的蒲蓝利咽合剂HPLC指纹图谱及绿原酸等8种成分的含量测定方法,可用于该制剂的质量评价;黄芩苷、汉黄芩苷、千层纸素A-7-O-β-D-葡萄糖醛酸等12种成分可能是影响蒲蓝利咽合剂质量的标志物。

Determination of anthraquinone prodrug and its hydrolytically active compounds using RP-HPLC

In order to study the hydrolytic characterization of an anti-inflammatory prodrug （ RI-1 ） in vitro, an effective, accurate and reliable method for the simultaneous determination of the prodrug and its two hydrolytic active compounds is developed using reverse phase high-performance liquid chromatography （RP-HPLC）. The chromatographic separation is performed on an ODS-2 C18 column （250 mm × 4. 6 mm, 5.0 μm particle size） with a simple elution program. The mobile phase is V（ methanol） ： V（0. 1% phosphoric acid solution） =90：10 （adjust pH to 2. 3）. A wavelength of 225 nm and a mobile phase flow rate of 1.0 mL/min are utilized for the quantitative analysis. Excellent linear behaviors over the investigated concentration ranges are observed with values of R2 higher than 0. 999 for all the analytes. The validated method is successfully applied to the simultaneous determination of the prodrug and its active components can be used to detect hydrolytic characterization in vitro.

Formulation, stability testing, and analytical characterization of melatonin-based preparation for clinical trial

A new institutional clinical trial assessed the improvement of sleep disorders in 40 children with autism treated by immediate-release melatonin formulation in different regimens(0.5 mg, 2 mg, and 6 mg daily) for one month. The objectives of present study were to(i) prepare low-dose melatonin hard capsules for pediatric use controlled by two complementary methods and(ii) carry out a stability study in order to determine a use-bydate. Validation of preparation process was claimed as ascertained by mass uniformity of hard capsules.Multicomponent analysis by attenuated total reflectance Fourier transformed infrared(ATR-FTIR) of melatonin/microcrystalline cellulose mixture allowed to identify and quantify relative content of active pharmaceutical ingredients and excipients. Absolute melatonin content analysis by high performance liquid chromatography in 0.5 mg and 6 mg melatonin capsules was 93.6% ± 4.1% and 98.7% ± 6.9% of theoretical value, respectively. Forced degradation study showed a good separation of melatonin and its degradation products. The capability of the method was 15, confirming a risk of false negative < 0.01%. Stability test and dissolution test were compliant over 18 months of storage with European Pharmacopoeia. Preparation of melatonin hard capsules was completed manually and melatonin in hard capsules was stable for 18 months, in spite of low doses of active ingredient. ATR-FTIR offers a real alternative to HPLC for quality control of highdose melatonin hard capsules before the release of clinical batches.

前胡和硬前胡化学模式识别及检验方法研究

目的通过高效液相色谱法(HPLC)测定前胡和硬前胡中白花前胡甲素和白花前胡乙素的含量,运用统计学方法对其进行质量分析比较和化学模式识别,并制定其检验方法。方法采用Waters SunFire C_(18)色谱柱(250 mm×4.6 mm,5μm);流动相为甲醇和水溶液,梯度洗脱,体积流量1.0 mL/min,检测波长320 nm。使用SPSS 26.0分析样品中白花前胡甲素和白花前胡乙素含量。结果前胡与硬前胡质量存在明显差异,白花前胡甲素和白花前胡乙素峰面积比值,前胡<1.0,硬前胡>1.0,可用于区别两种;前胡的指纹图谱相似度在0.85以上,硬前胡小于0.2;聚类分析中前胡和硬前胡各自相聚。结论所建立的方法可用于前胡和硬前胡的判别,操作快捷、简便和实用。

Content Determination of Five Kinds of Flavonoids in Trichosanthes Peel

[Objectives]The purpose of this study was to establish a method for the determination of five kinds of flavonoids in trichosanthes peel.[Methods]The contents of rutin,isoquercitrin,quercitrin,quercetin and kaempferol in trichosanthes peel samples collected from different sites were determined by high-performance liquid chromatography.With each component as an index,principal component analysis and cluster analysis were performed.[Results]The contents of flavonoids in the trichosanthes peel samples from different sites were different.The cumulative variance contribution rate of isoquercitrin was 95.514%.The results of cluster analysis show that the quality of trichosanthes peel from Anhui was the best.[Conclusions]Taking isoquercitrin as a common factor to carry out content determination will help to better control the quality of trichosanthes peel.

基于指纹图谱、化学模式识别及多成分定量的解酒保肝口服液质量评价研究

目的建立解酒保肝口服液的指纹图谱及多成分含量测定方法。方法采用高效液相色谱(HPLC)法和中药色谱指纹图谱相似度评价系统相似度软件建立11批解酒保肝口服液的指纹图谱,利用主成分分析(PCA)和偏最小二乘回归分析(PLS-DA)对解酒保肝口服液的质量进行分析研究;确定解酒保肝口服液中有效成分含量测定方法并测定其含量。结果建立了解酒保肝口服液HPLC指纹图谱,确定了29个共有峰,并指认检测了其中葛根素、毛蕊异黄酮苷、芦丁、木犀草苷、槲皮素5种有效成分。11批样品HPLC图谱相似度均大于0.950,PCA和PLS-DA找到了影响指纹图谱的6个主要成分,累计方差贡献率为92.89%,色谱峰24,29,22,23(木犀草苷),3,18,6,17,27,20,7,25,26,19(毛蕊异黄酮苷)的变量重要性投影(VIP)值>1,可作为解酒保肝口服液的质量差异性成分。11批解酒保肝口服液中葛根素、毛蕊异黄酮苷、芦丁、木犀草苷、槲皮素的质量浓度分别为106.698~236.795,0.815~1.868,14.552~16.662,8.204~13.12,18.731~20.427μg/mL。结论HPLC指纹图谱结合模式识别及多成分含量同时测定的方法为解酒保肝口服液提供了科学、可靠的质量评价方法,对解酒保肝口服液质量控制标准的建立具有重要意义,也为中药复方制剂的质量评价研究提供了参考。

基于UPLC指纹图谱、含量测定及化学识别模式的藏药多腺悬钩子质量评价研究

目的:建立多腺悬钩子的超高效液相色谱(UPLC)指纹图谱及含量测定的方法,结合化学模式识别分析,为其质量评价提供依据。方法:采用菲罗门Titank C_(18)色谱柱(100 mm×2.1 mm, 1.8μm),以0.1%磷酸-乙腈为流动相,梯度洗脱,流速0.4 mL·min^(-1),柱温40℃,检测波长254 nm,进样量3μL,建立多腺悬钩子UPLC方法,测定其中咖啡酸、鞣花酸、异槲皮苷的含量;基于指纹图谱共有峰峰面积结果,采用二维聚类分析、主成分分析、正交偏最小二乘判别分析、统计学分析、模式识别的化学计量学方法评价多腺悬钩子整体质量。结果:多腺悬钩子UPLC指纹图谱共确定16个共有峰;3个指标性成分在各自浓度范围内线性关系良好(r≥0.999 5),19批多腺悬钩子中咖啡酸、鞣花酸、异槲皮苷的含量分别为0.014%~0.118%,0.013%~0.120%和0.012%~0.374%。33批悬钩子聚为4类,可区分不同的悬钩子;主成分分析得到4个影响悬钩子分类的主要因子;正交偏最小二乘判别分析显示13号色谱峰的化合物、鞣花酸、咖啡酸、异槲皮苷、5号色谱峰的化合物、15号色谱峰的化合物可作为鉴别和区分多腺悬钩子与其他悬钩子的主要差异性标志物;统计学分析显示咖啡酸与异槲皮苷的含量差异是多腺悬钩子与粉枝莓的重要区别点;模式识别研究中所建模型可准确识别多腺悬钩子,预测结果较为理想。结论:所建立的方法稳定、可靠,能较全面地反映并评价多腺悬钩子的整体质量,为多腺悬钩子的质量控制提供参考。

藿香正气水快速质量评价(Ⅰ)——化学计量学辅助的UPLC指纹图谱研究

目的研究藿香正气水的快速质量评价方法。方法采用超高效液相色谱建立指纹图谱,并进行方法学考察。与对照品、药材和对照提取物比较,确定特征峰及其归属。测定13个厂家的28批产品,直观分析其指纹图谱的异同,进一步使用二维聚类分析和主成分分析进行模式识别。结果 18个特征峰主要与厚朴、陈皮、白芷、甘草浸膏、苍术、广藿香油相关,不同厂家的藿香正气水UPLC指纹图谱存在明显差异。聚类分析和主成分分析结果基本一致,样品按厂家各自聚为一类,和厚朴酚、厚朴酚、橙皮苷特征峰对指纹图谱影响最大。结论化学计量学辅助的UPLC指纹图谱具有快速、简便、客观、可数字化的优点,为藿香正气水的质量评价提供了一种新的思路。