目的:采用在线中心切割超高效二维液相色谱(2D-UPLC)法,建立同时测定复方南星止痛膏中3个双酯型乌头生物碱(新乌头碱、乌头碱和次乌头碱)的含量测定方法.方法:一维UPLC采用Waters XBridgeBEH C18色谱柱(2.1 mm×50 mm 1.7 μm),以甲醇-0.008％二乙胺为流动相,梯度洗脱,流速0.1 mL· min-1,柱温18℃;二维UPLC采用Waters XBridge BEH C18色谱柱(3.0 mm×100 mm 1.7 μm),以乙腈-0.01％磷酸为流动相,梯度洗脱,流速0.7 mL· min-1,柱温40℃.进样量1μL,检测波长235 nm.结果:新乌头碱、乌头碱和次乌头碱的线性范围分别为0.66～9.90、0.55～8.20和0.91～13.72 μg· mL-1,R2分别为0.999 5、0.999 9和0.999 6,线性关系良好;3个成分的平均加样回收率在82.5％～88.8％之间,方法的准确度和稳定性均较好;复方南星止痛膏中新乌头碱、乌头碱和次乌头碱含量分别在3.2～5.0、0.9～1.3、8.5～10.4 μg· g-1范围内.结论:该方法有效改善了复方南星止痛膏中待测组分的分离度,极大提高了检测灵敏度,对制剂中的3个双酯型乌头生物碱进行准确定量分析,提高产品的质量控制水平,并为临床用药提供理论支持.

目的 建立栀子的指纹图谱并采用电喷雾离子源-四极杆-飞行时间质谱(ESI-Q-TOF MS)对其共有峰进行定性分析.方法 采用Kromasil 100-5 C18柱,以乙腈-0.1％磷酸梯度洗脱,体积流量为1mL/min,柱温为35℃,检测波长为238、327、440 nm.使用Matlab 7.1软件编程,对3波长下的CSV格式数据进行全时段融合.结果 各色谱峰分离度良好,3波长融合指纹图谱全面体现了栀子238、327、440 nm特征吸收波长的指纹信息,标定20个共有峰,并完成其中16个成分的鉴定.10批不同批次的栀子指纹图谱与对照指纹图谱之间相似度较好,相似度大于0.90以上.结论 实现了栀子融合指纹图谱的测定,同时解析了图谱中的化学组成,并制定了主成分与栀子苷相对峰面积的范围,为全面控制药材质量提供了数据支撑.

Objective To establish an HPLC fingerprint of the compounds in Qibai Pingfei Granules (QPG),and to make a quantitative analysis.Methods Sample was extracted by 50％ methanol.Phenomenex Luna C18 column (250 mm × 4.6 mm,5 μm) was used with a mobile phase of methanol-0.2％ formic acid gradient elution.The flow rate was 1.0 rnL/min,the detection wavelength was 250 nm,and the column temperature was 30 ℃.The chemical component fingerprint similarity of 10 batches of QPG was calculated with Chinese Medicine Chromatographic Fingerprint Similarity Evaluation System (2012) published by National Pharmacopoeia Committee and the common peaks were identified by reference compounds.Results Fingerprints of 10 batches of QPG were established and the similarities to the common mode were above 0.96.Totally 25 common peaks were found.Among them,peak 1 belonged to Pheretima,peaks 2 and 3 belonged to Pheretima and Ginseng Radix et Rhizoma (GRR),peak 4 belonged to GRR,Schisandrae Chinensis Fructus (SCF),and Chuanxiong Rhizoma (CR),peak 5 belonged to GRR,Allii Macrostemonis Bulbus (AMB),CR,and Pheretima,peaks 6,8,22,23,24,and 25 belonged to SCF,peak 7 belonged to Astragali Radix (AR) and SCF,peak 9 belonged to GRR and AMB,peak 10 belonged to Descurainiae Semen Lepidii Semen (DSLS) and AMB,peaks 11,12,13,15,and 16 belonged to CR,peak 14 belonged to AR and DSLS,peaks 17,18,19,20,and 21 belonged to AR.Based on the retention time,and UV absorption spectra of reference compounds,six constituents including caffeic acid (peak 12),ferulic acid (peak 13),schizandrol A (peak 22),schisantherin A (peak 23),deoxyschizandrin (peak 24),and schisandrin (peak 25) were identified.The linear ranges of caffeic acid,ferulic acid,schizandrol A,schisantherin A,deoxyschizandrin,and schisandrin were 3.38-108.02,3.60-115.33,2.99-95.61,2.81-89.77,3.26-104.17,and 2.89-92.45 μg/mL,respectively.In 10 batches of QPG samples,the contents were as follows:caffeic acid of 0.412-0.429 mg/g,ferulic acid of 0.302-0.317 mg/g,schizandrol of A 0.182-0.195 mg/g,schisantherin A of 0.179-0.195 mg/g,deoxyschizandrin of 0.203-0.215 mg/g,and schisandrin of 0.131-0.144 mg/g,the amount of each indicator composition among different batches changed a litte,and the sample quality is stable.Conclusion The method has good precision,reproducibile,stability,separation,and can be used for the quality control of QPG.

目的 建立银翘清热片(YQT)的HPLC指纹图谱,并采用电喷雾离子源-四极杆-飞行时间质谱(ESI-Q-TOF/MS)对其化学成分进行定性分析.方法 采用Kromasil C18柱(250 mm×4.6 mm,5μm),以乙腈-0.1％磷酸水溶液梯度洗脱,体积流量为1 mL/min,柱温为25℃,检测波长为230 nm.ESI-Q-TOF/MS正、负2种离子模式扫描对其化学成分定性分析.结果 建立了YQT HPLC指纹图谱,标定28个共有峰,归属到6味药材,其中7个共有峰来源于连翘,9个共有峰来源于金银花,6个共有峰来源于葛根,3个共有峰来源于牛蒡子,1个共有峰(2号)来源于连翘和升麻,另外2个共有峰分别来源于知母和升麻.11批不同批次的YQT制剂相似度均大于0.95.并采用LC-Q-TOF/MS方法鉴定了42个化学成分,其中16个采用对照品比对鉴定,分别为葛根素、大豆苷、大豆苷元、新绿原酸、绿原酸、隐绿原酸、异绿原酸A、异绿原酸B、异绿原酸C、断氧化马钱苷、芦丁、连翘苷、连翘酯苷A、牛蒡苷、芒果苷、知母皂苷B Ⅱ.结论 完善了YQT的质量标准体系,可为同类型的其他复方制剂的物质基础研究和质量控制提供参考.

为了提高银翘清热片的质量标准，建立了制剂中连翘、牛蒡子、知母和升麻的薄层定性分析方法，并采用反相液相色谱法测定了绿原酸、连翘苷和牛蒡苷的含量。试验结果证明，在选定的薄层色谱条件下，色谱斑点清晰，分离效果较好，且无阴性干扰。所建立的方法准确、灵敏、简便，重复性好，能更好地控制银翘清热片的质量。

In this article, an HPLC method for the contents determination of amino acids in Qihong Maitong injection was reported. In detailed, OPA-Fmoc pre-column derivatization was adopted, and related HPLC methods to determine the contents of amino acids was established. Linear relationship was well constructed for 17 amino acids through the method mentioned above. Briefly speaking, the optimized method was accurate and reproducible, and suitable for the determination of amino acids in Qihong Maitong injection and corresponding quality control.

HPLC fingerprint of Congrong Zonggan capsule was established in order to provide basis for quality evaluation. With acteoside as the reference, HPLC was adopted for fingerprint analysis on Congrong Zonggan capsule. The chromatographic conditions wereas follows. Waters C18 column (4.6 mm x 150 mm, 5 μm) was used, with methylalcohol-0.1% formic acid as the mobile phase for gradient elution at the flow rate of 1.0 mL x min(-1). The detection wavelength was 330 nm, and the column temperature was 30 °C. This method was highly accurate and reproducible. All of the 13 components in tested samples reached the baseline resolved peak, and 15 batches of finished products showed the similarity of above 0.95. The method was accurate and feasible and could be used as a simple and effective method to evaluate the quality of the traditional Chinese medicines.

介绍了滚模式软胶囊制丸机的结构、工作原理及其在中药制剂生产中的应用,结合滚模式软胶囊制丸机的特点,分析了设备运行过程中的常见问题,并提出了相应的解决措施,为企业提高工作效率提供了参考。

Objective To optimize the impurity removal technology before ultrafiltration,taking Qihong Maitong Injection(QMI) as the research object.Methods The removal of impurities and related substances by the combined process of refrigeration,centrifugation,and activated carbon adsorption was investigated.Taking the contents of total saponins of astragalus,astragaloside,and hydroxy safflower yellow pigment A,solids reduction efficiency,protein concentration,and related substances inspection as the evaluation indexes,the feasibility of the impurity removal method was definited and the process parameters were optimized.Results The optimized process parameters were as follows: refrigerated for 24 h,centrifugated for 15 min,at 5 000 r/min,activated carbon dosage of 0.3%,temperature 40 ℃,adsorption time 30 min,and the original solution pH value.Conclusion The impurity removal effect of refrigeration,centrifugation,and activated carbon adsorption is significant,which could effectively remove the resin,protein,and other impurities.

目的 建立散结镇痛胶囊中皂苷类成分的HPLC指纹图谱.方法 经水饱和正丁醇提取后,用氢氧化钠溶液萃取,采用D-101大孔树脂富集制备供试品溶液.色谱条件为Waters Symmetry@C18 (250 mm×4.6 mm,5 μm)色谱柱；流动相为乙腈-水,梯度洗脱;检测波长203 nm;体积流量1.0 mL/min;柱温30℃.采用国家药典委员会出版的《中药色谱指纹图谱相似度评价》(2004年A版)软件,对11批不同批次的散结镇痛胶囊中皂苷类成分指纹图谱进行相似度计算.结果 11批散结镇痛胶囊指纹图谱中有9个共有峰,各峰分离度良好,各批次间共有峰的相对保留时间RSD均＜1.0％,样品间相似度均＞95％.结论 本方法具有良好的精密度、重现性、稳定性,各共有峰间分离度高,可用于散结镇痛胶囊质量综合评价.

Objective:To establish the chromatographic fingerprint analysis for the quality control of the content of flavonoids in Sanjie Zhentong capsules.Method: Under the operation of ultrasonic extraction,the flavonoids from Sanjie Zhentong capsules were extracted in the 50% methanol.With Waters Symmetry@ C18(4.6 mm×250 mm,5 μm)column,and gradient elution was performed by mobile phase containing acetonitrile and water.The flow rate was 1.0 mL·min-1 and the detection wave length was at 203 nm.The temperature of column was maintained at 30 ℃.And data were analyzed by 'Similarity evaluation software for chromatographic Fingerprint of traditional Chinese medicine' software to compare the quanlity of 11 batches of capsules samples.Result: Fifty common peaks were selected in chromatography,and all the common peaks were separated effectively.Conclusion: The accuracy,repeatability,and stability of this method were satisfied.The method developed can be used to evaluate the quality of Sanjie Zhentong capsules synthetically.

目的 优选玄参脑保护作用提取物最佳水提醇沉工艺.方法 采用正交试验,以干膏率,哈巴苷和哈巴俄苷转移率为指标,对玄参水提醇沉工艺进行优化；并考察了醇沉前后的样品对大鼠缺血脑组织的保护作用.结果 优选的最佳水提醇沉工艺为:8倍热水浸泡1 h,提取3次,每次1.5 h,再将提取液浓缩至相对密度1.15,调节醇量为60％,静置36h.且纯化后的玄参提取物对大鼠缺血脑组织仍有良好的保护作用.结论 优选的工艺稳定,可行.

The method of preparing Ginkgolides gastric floating sustained-release tablet was studied and the releasing characteristics in vitro were also investigated.The floating and releasing performance in vitro were used as indicators to evaluate and optimize the formulation.Effects of hydroxypropyl methyl cellulose(HPMC) type and amount,sodium bicarbonate amount and stearic acid amount on release behavior in vitro were observed in single-factor testing method.Then the formulation was optimized by orthogonal design test to determine the best preparation technological conditions.The result showed that gastric floating sustained-release tablets,which were prepared with HPMCK4M as matrix,stearic acid as floating assistant,sodium bicarbonate as gas-producer,and microcrystalline cellulose and lactose as fillers,was taken once a day.And the tablet was released 35% in 2 h,60% in 6 h,exceeding 85% in 12 h.The releasing rate met requirements for gastric floating sustained-release.It is concluded that ginkgolides gastric floating sustained-release tablets prepared in this method has good release characteristics.The tablets are in good shape and compressibility.The preparative technology is also simple with low manufacture cost.

Objective:To establish an HPLC method for determination of protopine and tetrahydropalmatine in Tongning Gel.Method:The liquid chromatography was carried out using Kromasil C18(4.6 mm × 250 mm,5 μm),with detection wave length at 280 nm,acetonitile-phosphate buffer as mobile phase,gradient elution.The column temperature was at 30 ℃ and the flow rate was 1.0 mL·min-1.Result:The calibration curve of protopine was linear in the range of 0.100 6-5.03 μg(r = 1),and the recovery was 99.14%(RSD 1.34%).The calibration curve of tetrahydropalmatine was linear in the range of 0.100 8-5.0 4 μg(r = 1),and the recovery was 101.1%(RSD 1.18%).Conclusion:This method is simple,accurate,reliable and reproducible,which can be used for quality control of Tongning Gel.

This study aimed to investigate the influence of reusing time of D101 macroporous resin on the adsorption rate of HSYA A in order to provide basis for industrial production.Static adsorption was used in the study on attenuation of repeated regeneration D101 macroporous resin.High Performance Liquid Chromatography(HPLC) was applied in the quantitative analysis of HSYA A contents.The results showed that through the repeated regeneration processed by ethanol,2% hydrochloric acid and 5% sodium hydroxide,after 16 times using,the adsorption rate of D101 macroporous decreased by about 27%.It is concluded that D101 macroporous resin after regeneration and reactivation can be used for no more than 16 times.

目的 测定芪葛口服液中主要成分黄芪甲苷.方法 采用HPLC-ELSD法.色谱柱为Agilent Zorlpax-C18柱(150 mm×4.6 mm,5μm),流动相为乙腈-水(33:67),柱温30℃,体积流量1 mL/min,蒸发光散射检测漂移管温度43℃,雾化器温度35℃,氮气压力172 kPa;进样量5μL.结果 黄芪甲苷在1.012～10.120μg具有良好的线性关系,平均加样回收率为96.89%,RSD为1.58%.结论 本方法简便、快捷、重现性好,适用于芪葛口服液的质量控制.