鱼腥草芩蓝口服液质量控制方法研究

为建立鱼腥草芩蓝口服液的质量控制方法,采用TLC法对鱼腥草芩蓝口服液中的鱼腥草、黄芩、连翘和金银花进行鉴别;采用HPLC法测定黄芩苷和绿原酸的含量。在薄层色谱鉴别中均能检出鱼腥草、黄芩、连翘和金银花的特征性斑点;黄芩苷进样量在0.1057～2.6413μg范围内与峰面积有良好的线性关系,回归方程为:Y=33.42325X-214.6128,r=0.9997,平均回收率为98.74%;绿原酸进样量在0.041～2.051μg/m L范围内与峰面积有良好的线性关系,其回归方程为:Y=-86.78088+27.5937X,相关系数r=0.9995,回归显著,平均回收率为99.1%,建立的黄芩苷和绿原酸含量测定方法,耐受性良好、灵敏度高、重现性好、专属性强,可以有效控制产品的质量。建立的方法能准确、可靠地对鱼腥草芩蓝口服液中黄芩苷和绿原酸含量进行测定,可作为该制剂的质量控制方法。     

HPLC测定银黄颗粒中绿原酸和黄芩苷的含量

为准确测定银黄颗粒制剂中绿原酸和黄芩苷的含量,建立了一套运用HPLC进行绿原酸和黄芩苷含量测定的简便方法。色谱柱,十八烷基硅烷基键合硅胶柱（4．6mm×250mm;5μm）;绿原酸检测波长为327nm;流动相,乙腈-0．4％磷酸溶液（10：90）;黄芩苷检测波长为274nm;流动相,甲醇-水-0．29／6磷酸（50：50：0．2）,并对该方法进行了方法学考证。结果表明,此方法具有样品处理简便、色谱分离度和重现性好的特点,可用于银黄颗粒制剂中绿原酸和黄芩苷含量的准确测定,以实现对银黄颗粒产品的质量控制。     

正交设计法优选黄芩苷的提取工艺研究

本研究采用煎煮法提取黄芩中的黄芩苷,运用紫外分光光度法对黄芩苷的含量进行测定,分析提取次数、料液比和提取时间等因素的影响,并在此基础上进行正交试验,优化提取工艺参数。结果表明:当提取次数为2次,料液比为1:25,每次煎煮50 min时,黄芩苷的提取效果最好,提取率为20.36%。该优化工艺条件稳定、可靠,可作为工业化生产黄芩苷的理论依据。     

HPLC同时测定中药复方“LH”中绿原酸和连翘苷的含量

目的：建立同时测定中药复方“LH”中绿原酸和连翘苷含量的高效液相色谱方法。方法：以Zorbax Extend．C18柱（4．6mm×150him,5μm）为色谱柱,以乙腈-0．1％醋酸溶液为流动相,梯度洗脱,流速1．0mL／min,检测波长344nm。结果：绿原酸、连翘苷的线性范围分别为0．0125—0．625vg（r=0．9999）,0．05—2．5μg（r=0．9999）,平均回收率为98．40％和96．67％,RSD分别为1．35％、1．23％（n=6）;结论：该法准确、快速、简便、重现性好,且具有良好的回收率,可用于中药复方“L”中绿原酸和连翘苷的含量测定。     

清解合剂提取工艺优化

优化清解合剂的提取工艺,充分提取药物中的有效成分。采用单因素试验确定不同因素对提取工艺的影响以及正交试验的因素与水平;用高效液相色谱检测黄芩苷的含量,以黄芩苷含量和干膏得率为综合评价指标,采用加权评分法进行综合评分,筛选出清解合剂的最佳提取工艺。结果表明,最优提取工艺为料液比1∶15(g∶mL),提取时间1 h,提取次数2次,黄芩苷的线性回归方程为y=37 499x-112 622(R2=0.999 6),黄芩苷对照品质量浓度在7.81～500.00μg/mL范围内呈现良好的线性关系。表明优选的提取工艺稳定可行,为规模化生产提供一定的理论依据。     

玉米秸秆及其青贮饲料干物质降解率相关分析

本研究利用安装有永久性瘤胃瘘管的西门塔尔杂种阉公牛,应用尼龙袋技术,测定了玉米尊秆及其相应青贮饲料的干物质瘤胃降解变化,并进行相关分析。试验结果表明：秸秆干物质瘤胃降解率（X）与秸秆青贮干物质瘤胃降解率（Y）二者间存在强正相关关系（P〈0．01）,回归方程为：Y=0.4718＋1．1620X（r2=0．9835,n=5）。     

高效液相色谱法测定双黄败毒颗粒中黄芩苷含量

采用RP—HPLC法测定双黄败毒颗粒中黄芩苷的含量。样品用70％乙醇超声处理，以C18为固定相，甲醇-水-磷酸（45：55：0．2）为流动相，280nm为检测波长，用HPLC法测定其中黄芩苷含量。黄芩苷的线性范围为0．16—0．96μg，r=0．9997（n=6），平均加样回收率为102．2％，RSD为1．57％（n=9）。     

HPLC法测定黄芩苷-β-环糊精包合物中黄芩苷的含量

为了建立HPLC法测定黄芩苷-β-环糊精包合物中黄芩苷的含量方法,在CLC-ODSC18柱上,以甲醇-水-磷酸(47:53:0.2)为流动相,检测波长280 nm,以外标法定量测定了黄芩苷-β-环糊精包合物黄芩苷的含量.结果:线性范围为20.0～80.0μg/ml,回归方程为Y=9753.1X 1546,r=0.9993(n=5),平均加样回收率为99.37%(n=5),精密度试验RSD为0.30%(n=6).本方法准确、可靠、重现性好,可作为黄芩苷-β-环糊精包合物中黄芩苷的含量测定方法.     

HPLC波长切换法同时测定双黄连可溶性粉中3个成分的含量

目的:建立HPLC波长切换法同时测定双黄连可溶性粉中绿原酸、黄芩苷、连翘苷3种成分的含量测定方法。方法:采用Waters XSelect CSH C_(18)(4.6 mm×250 mm,5μm),以甲醇(A)-0.1%磷酸水溶液(B)为流动相,梯度洗脱,流速1 mL/min,测定绿原酸、连翘苷、黄芩苷的检测波长分别为326 nm(0～26 min)、230 nm(40～43 min)、277 nm(43～46 min)。结果:各待测组分分离度良好;绿原酸、连翘苷、黄芩苷3种成分的进样量分别在0.045 3～0.453 0μg(r=0.999 7),0.027 8～0.278 0μg(r=0.999 4),0.219 0～2.190 0μg(r=0.999 9)与峰面积呈良好的线性关系;加样回收率(n=6)分别为98.0%(RSD=1.8%)、100.8%(RSD=2.0%)、99.3%(RSD=1.0%)。结论:本试验建立的含量测定方法符合方法学验证要求,可用于双黄连可溶性粉的3个指标性成分的同时测定。     

高效液相色谱法测定胆翘注射液中黄芩苷的含量

采用高效液相色谱法测定胆翘注射液中黄芩苷的含量[1]。色谱柱为Agilent Eclipse XDB-C18(5μm,250mm×4.6mm id),流动相为甲醇—水—冰乙酸(50∶50∶1),检测波长为274nm,流速1.0mL/min,柱温30℃。在相同的色谱条件下,探讨50%甲醇溶剂、流动相(50∶50∶1)对含量测定的影响,实验结果表明,不干扰黄芩苷含量结果测定(见图1、图2)。黄芩苷在0-100μg/mL浓度范围内线性关系良好R2=0.9999(n=6),回归方程为y=19.7840X+4.9103,回收率为97.6%~98.9%,相对标准偏差为0.5%。本方法简单、准确、可行,适用于胆翘注射液中黄芩苷含量测定。     

鸡血浆中黄芩苷及绿原酸的HPLC法建立

建立了测定鸡血浆中复方慢呼抗口服液主要成分黄芩苷和绿原酸的高效液相色谱法.流动相为乙腈、1％冰醋酸,梯度洗脱30 min,黄芩苷和绿原酸的波长分别为280、327 nm,流速1 mL/min.分别采用高氯酸法、甲醇乙腈法、正丁醇法处理血浆,选取最优方法进行考察.甲醇乙腈法处理血浆,方法专属性好,回收率较高,线性关系良好,精密度及准确度较高,可用于药代动力学研究.     

复方茜草灌注液质量标准研究

目的：制定复方茜草灌注液质量标准。方法：采用薄层色谱法对制剂中的丹参、茜草、苦参进行鉴别;采用高效液相色谱法测定制剂中丹参酮ⅡA和隐丹参酮的含量。结果：隐丹参酮的回归方程Y=1×106 X＋744 462,r=0.999 5,平均回收率为98.5%,RSD为1.61%。丹参酮ⅡA的回归方程Y=2×106 X＋2×106,r=0.999 5,平均回收率为97.8%,RSD为2.05%。结论：建立的鉴别方法直观、简单、专属性强;含量测定方法准确、重现性好。可作为制定复方茜草灌注液质量标准的试验依据。     

HPLC法测定徐长卿中绿原酸的含量

建立HPLC法测定徐长卿中绿原酸的含量。采用索氏提取法以70％的甲醇水溶液为提取剂对徐长卿中的绿原酸进行提取。在SHIMADZU C18色谱柱（250mm×4．6mm,5μm）,流动相乙腈-0．5％磷酸水溶液（1：9,V/V）;流速1．0mL/min;柱温25℃;检测波长327nm的条件下进行检测。结果表明,绿原酸在0．232—4．640μg范围内与峰面积呈良好线性关系,r=0．9997。平均回收率为99．32％,RSD为0．216％（n=5）。该方法简便、可靠、重现性好,可作为徐长卿中绿原酸含量测定的方法。     

Prediction of crude fat content of longissimus muscle of beef using the ratio of fat area calculated from computer image analysis: comparison of regression equations for prediction using different input devices at different stations

Crude fat content of longissimus (ribeye) muscle of beef cattle was predicted from a ratio of fat area (RFA) to area of ribeye muscle calculated from computer image analysis (CIA). Cross sections of 64 ribeyes taken from the 6-7th rib from cattle at experiment station A and cross sections of 94 ribeyes taken from the 6-7th rib from cattle at Experiment Station B were used in this study. Slices (1 to 1.5 cm in thickness) of just the Longissimus dorsi were homogenized and sampled for chemical estimation of crude fat content using petroleum ether. Crude fat content as determined from chemical analysis was used as the true estimate of fat content. A CCD (charge-coupled device) camera was used as the input device at Experiment Station A, and a single-lens reflex camera was used at Experiment Station B to photograph ribeyes for CIA. The contour comparison method, which assigns a threshold value for each marbling particle, was used to obtain accurate binarization in this study. Minimum and maximum of chemical measurements of crude fat were 2.1 and 39.8%, and for CIA calculation of the RFA were 6.1 and 56.8%, respectively. This range covered almost the complete range of the beef marbling standard used in carcass grading in Japan. The equation for the regression of the crude fat content (Y) on RFA (X) calculated from CIA for all of the data was Y = .793X-3.04 with r2 = .96. Regression equations for prediction of crude fat percentage from RFA taking into consideration the effect of experiment station were Y = .741X-2.22 with r2 = .91 for Experiment Station A, and Y = .782X-2.54 with r2 = .91 for Experiment Station B. Analysis of covariance showed that the effects of experiment stations on intercepts and slopes were not significant (P > .10). The ranges of differences between actual and predicted crude fat content from the prediction equation that was calculated without consideration of the effect of station were -6.4 to 4.0%. CIA of cross sections of the ribeye muscle seems to have potential for prediction of crude fat content.     

复方中药软膏剂的透皮效果研究

为评价中药复方软膏剂透皮效果,筛选最佳组方,以中药软膏剂中绿原酸成分为标记物,应用高效液相色谱法(HPLC)测定透过液中绿原酸的含量,评价不同的中药剂型和不同的透皮促渗剂对中药软膏剂透皮效果的影响。结果表明,中药超微粉直接入药并以含45 g/L冰片+45 mL/L氮酮作为促渗剂效果最佳。     

银翘药对注射液在家兔体内的药动学

为了考察银翘药对配伍的科学性,利用高效液相色谱法分析检测了金银花注射液(A)、连翘注射液(B)、银翘药对注射液(C)以及金银花注射液、连翘注射液的混合液(D)主要成分绿原酸、连翘苷在家兔体内的药动学过程。结果A、C、D 3种注射液肌注后绿原酸在家兔体内药动学过程符合二室模型,其Cmax分别为:1.567、1.656、1.612 g.L-1;Tmax分别为:0.413、0.224、0.285 h;Tβ/2分别为1.164、1.227、1.132 h;AUC分别为1.905、2.623、2.114 mg.h.L-1;B、C、D 3种注射液肌注后连翘苷在家兔体内药动学过程符合一室模型,其Cmax分别为1.548 g.L-1、1.902、1.576 g.L-1;Tmax分别为:0.742、0.606、0.646 h;Tβ/2分别为1.272、1.212、1.220 h;AUC分别为2.80、3.216、2.881 mg.h.L-1。试验结果经统计学分析,配对能缩短绿原酸达峰时间Tmax,混合煎煮能提高连翘苷药峰浓度Cmax;配对并混合煎煮2种成分的药时曲线下面积(AUC)均显著提高,说明银翘配对并混合煎煮具有其科学依...     

乳腺康注射液质量标准研究

本研究旨在建立乳腺康注射液质量标准。按照《中国药典》（2015版）相关要求,分别建立乳腺康注射液中甘草、青皮、蒲公英的薄层色谱定性鉴别和重金属的检查方法并规定限度,采用HPLC法建立甘草苷、甘草酸铵、橙皮苷及咖啡酸的含量测定方法并规定限度。结果表明,甘草、青皮、蒲公英的定性鉴别专属性强;甘草苷在0.0459~0.7340 μg,甘草酸铵在0.0661~1.0580 μg,橙皮苷在0.0592~0.9470 μg,咖啡酸在0.0384~0.6140 μg浓度与峰面积呈良好的线性关系;相关系数r分别为0.997、0.9990、0.9999、1.000;甘草苷、甘草酸铵、橙皮苷及咖啡酸的平均加样回收率分别为101.25%、99.87%、98.39%、103.49%,相对标准偏差（RSD）值分别为4.82%、3.63%、2.94%、0.85%;乳腺康注射液中含甘草苷、甘草酸铵、橙皮苷及咖啡酸分别不低于88.90、138.48、136.50、21.54 μg/mL;按乳腺康注射液每日最大使用剂量计算,铅、镉、砷、汞、铜分别不得超过23、3、6、2及150 μg。本研究建立的质量标准可为控制乳腺康注射液的质量提供参考。     

Study on Quality Standard of Ruxiankang Injection

The aim of this study was to establish the quality standard of Ruxiankang (RXK) injection. According to the relevant requirements of the Chinese Pharmacopoeia (2015 edition), TLC identification,related substances examination and heavy metal examination method of RXK injection were established and the limits were determined. HPLC method was used to establish the content determination method of liquiritin, ammonium glycyrrhizinate, hesperidin and caffeic acid, and determined the limit. The specificity of Glycyrrhizae Radix et Rhizoma, Citri Reticulatae Pericarpium and Taraxaci Herba was strong. Liquiritin in 0.0459 to 0.7340 μg, ammonium glycyrrhizate in 0.0661 to 1.0580 μg, hesperidin in 0.0592 to 0.9470 μg, caffeic acid in the 0.0384 to 0.6140 μg concentration showed a good linear relationship with peak area. The correlation coefficients were 0.997,0.9990,0.9999 and 1.000,respectively. The average recoveries were 101.25%, 99.87%, 98.39% and 103.49%,respectively. The RSD values were 4.82%, 3.63%, 2.94% and 0.85%,respectively. The contents of liquiritin, ammonium glycyrrhizinate, hesperidin and caffeic acid of RXK injection were not less than 88.90, 138.48, 136.50 and 21.54 μg/mL,respectively. According to the maximum daily dose of RXK injection, Pb,Cd, As, Hg and Cu should not exceed 23,3,6,2 and 150 μg, respectively. The quality standard established in this study could provide reference for controlling the quality of RXK injection.