盐酸多柔比星的高效毛细管电泳法分析

用高效毛细管电泳法测定盐酸多柔比星的含量。考察不同试验条件下盐酸多柔比星的胶束动电毛细管电泳行为。选择５０ｍｍｏｌ／Ｌ十二烷基硫酸钠，５０ｍｍｏｌ／Ｌ硼 溶液（ｐＨ８．７）含１０％乙腈为运行缓冲液，以β－萘磺酸钠为内标，于２３１ｎｍ波长处测定。在０．１７～０．８５ｇ／Ｌ的范围内呈良好的线性关系，ｒ＝０．９９９４，重现性实验ＲＳＤ为２．５％（ｎ＝５）。     

碘普罗胺非离子型造影剂的胶束动电毛细管电泳分析

考察了不同实验条件下碘普罗胺（Ｉｏｐｒｏｍｉｄｅ）非离子型造影剂的胶束动电毛细管电泳行为。用２５ｍｍｏｌ／ＬＳＤＳ、１０ｍｍｏｌ／Ｌ氯化钠、１５ｍｍｏｌ／Ｌ硼砂缓冲液、ｐＨ８．５，毛细管（３０ｃｍ×５０μｍ）于２５５ｎｍ波长处检测碘普罗胺含量，在１０～２００ｍｇ／Ｌ浓度范围内呈较好的线性关系。３种不同浓度下碘普罗胺的回收率（ｎ＝３）分别为９７．５％、９９．８％、１０１．３％，相对标准偏差分别为３．１％、１．５％、２．９％。     

高效液相色谱法测定兔血浆中羟基喜树碱的含量

采用高效液相色支测定兔血浆中羟基喜树碱的含量。色谱柱为Ｓｈｉｍｐａｃｋ ＣＬＣ－ＯＤＳ,流动相为甲醇－１０ｍｍｏｌ／Ｌ磷酸盐缓冲液（６０：４０,ｐＨ４．０）,检测波长３８２ｎｍ。血药浓度在５２￣１０４００ｎｇ／ｍｌ范围内呈线性关系Ｙ＝－２２９４＋５０．６０Ｘ,ｒ＝０．９９９４,最低检出浓度为２０ｎｇ／ｍｌ,方法回收率为１０３．０％,ＲＳＤ为２．９６％（ｎ＝３）,萃取回收率为６３．２％,ＲＳＤ为２．     

毛细管区带电泳法测定复方马来酸依那普利片中两组分含量

用毛细管区带电泳法同时测定复方马来酸依那普利片中两组分含量。以咖啡因为内标，２０ｍｍｏｌ／Ｌ硼砂—２０ｍｍｏｌ／Ｌ磷酸二氢钠（４９∶５１，ｐＨ８６）为运行缓冲液，在７ｍｉｎ内完成分离。马来酸依那普利和氢氯噻嗪的线性范围分别为８０～６４０μｇ／ｍＬ（ｒ＝０９９９９）和５０～４００μｇ／ｍＬ（ｒ＝０９９９３）。平均回收率分别为１０１０％和１０１１％，ＲＳＤ分别为１０％和１７％，ｎ＝５。     

离子对高效液相色谱法测定人本血浆中阿昔洛韦的浓度

本介绍离子对高效液相色谱法测定人体血浆中阿昔洛韦浓度的方法，使用ＳｐｈｅｒｉｓｏｒｂＣ１８（Ｉ．Ｄ４．６×１５０ｍｍ）色谱柱，流动相组成为１ｍｍｏｌ／Ｌ十二烷基磺酸钠溶液（含５ｍｍｏｌ／Ｌ三氯乙酸）－乙腈（２０：１）检测波长为２５４ｎｍ，线性范围为０～１０００ｎｇ／ｍｌ，γ＝０．９９９８（ｎ＝８）平均回收率为１０１．２％ＲＳＤ为５．５１９％，本法具有简便，灵敏，准确等特点。     

高效液相色谱法测定维生素K3制剂含量的研究

本文建立反相高效液相色谱法测定制剂中维生素Ｋ３的含量，在ＯＤＳ柱上，以含１５ｍｍｏｌ／Ｌ磷酸二氢钠的甲醇－水（３０：７０）为流动相。测得维生素Ｋ３注射剂的回收率为９９．８％，ＲＳＤ为０．４５％，片剂的回收率为９９．７％，ＲＳＤ为０．４９％。本法简便，准确，适用于常规分析。     

毛细管电泳法测定盐酸西替利嗪糖浆中西替利嗪的含量

目的：建立毛细管电泳法测定盐酸西替利嗪糖浆剂中西替利嗪含量的方法。方法：以３０ｍｍｏｌ／Ｌ磷酸二氢钠（ｐＨ２．７）缓冲液为运行缓冲液,运动电压为２０ｋＶ,检测波长为２３０ｎｍ。结果：盐酸西替利嗪在６０￣１４０μｇ／ｍｌ浓度范围内有良好的线性关系（ｒ＝０．９９９３）,回收率为９８．４％,ＲＳＤ＝１．８％（ｎ＝６）。结论：毛细管电泳法可用于盐酸西替利嗪糖浆剂中西替利嗪的定量测定。     

左氧氟沙星注射剂含量及有关物质的HPLC测定

以反相高效液相色谱法测定左氧氟沙星注射剂的含量及有关物质。采用Ｗａｔｅｒｓ Ｎｏｖａ－ＰａｋＣ１８柱,１０ｍｍｏｌ／Ｌ ＫＨ２ＰＯ４－１０ｍｍｏｌ／Ｌ溴化四丁铵－乙腈（４５：４５：１０,磷酸调节ｐＨ２．８）为流动相,检测波长为２９３ｎｍ。平均回收率为１００．５％,ＲＳＤ为０．７１％。方便简便、准确。     

超氧化物歧化酶脂质体的制备

用均匀设计法优化ＳＯＤ脂质体（Ｌ－ＳＯＤ）的制备工艺；制得包封率为６４．５２±３．３５％、粒径为０．０４～１．０μｍ的Ｌ－ＳＯＤ。并发现将此Ｌ－ＳＯＤ分散于１０ｍｍｏｌ／ＬＰＢＳ（含０．１５ｍｏｌ／ＬＮａＣｌ，ｐＨ７．４０）中比较稳定，在４℃避光密封贮存６个月，其ＳＯＤ活性存留率仍在７０％以上。     

产青霉素酰化酶的大肠杆菌ATCC11105在两水相系统中的动力学…

本文研究了产青霉素酰化酶的大肠杆菌ＡＴＣＣ１１１０５在ＰＥＧ２００００－ＤｅｘｔｒａｎＴ７０两水相系统中的动力学行为，并与在磷酸盐缓冲液中的动力学行为进行了对照。产青霉素酰化酶的菌体在两水相体系中Ｋｍ值为４．３５ｍｍｏｌ／Ｌ，最适温度为５５℃，最稳定ｐＨ值为６．０－７．０，最稳定温度为３０℃；在磷酸盐缓冲液中Ｋｍ值为７．２０ｍｍｏｌ／Ｌ，最适ｐＨ值为８．０，最适温度为６５℃，最稳定ｐＨ值为８．０，     

毛细管电泳分析7-氨基头孢霉烷酸生产过程

建立了高效毛细管电泳分析法检测7-氨基头孢霉烷酸生产过程.采用未涂层石英毛细管柱,缓冲液为0.01mol/L磷酸盐缓冲液(pH 8.0),运行电压30kV,检测波长254nm.7-氨基头孢霉烷酸、头孢菌素C和戊二酰基-7-氨基头孢霉烷酸的线性范围(mg/ml)分别为0.05～3(r=0.998)、0.1～3.5 (r=0.992)和0.1～5 (r=0.996),迁移时间和峰面积的RSD分别为0.5%、1.0%、0.6%和2.2%、3.0%、2.4%.     

复方布洛芬软胶囊中2组分溶出度的测定方法研究

目的 :建立同时测定复方布洛芬软胶囊中布洛芬和对乙酰氨基酚2组分溶出度的方法。方法 :以磷酸盐缓冲液 (pH=7 2)为溶剂 ,转速为75r/min ,取样时间为45min ,采用反相高效液相色谱法测定布洛芬和对乙酰氨基酚的溶出度 ,其中色谱柱为氰基柱 ,流动相为磷酸盐缓冲液 (pH=6 6) -甲醇 (60∶40) ,流速为1 0ml/min ,检测波长为223nm ,柱温为30℃。结果 :对乙酰氨基酚与布洛芬检测浓度线性范围分别为0 17～100 14μg/ml(r=0 9999 ,n=9)、0 21～124 86μg/ml(r=0 9999 ,n=9) ;平均回收率分别为99 62 %(RSD=0 36 %)、99 79 %(RSD=0 49 %)。结论 :本方法简便、快速、准确、可靠 ,能同时测定复方布洛芬软胶囊中2组分的溶出量。     

HPLC法和UV分光光度法测定阿奇霉素片溶出度的方法比较

目的采用HPLC和UV分光光度法测定阿奇霉素片溶出度,并从中选择适宜的方法。方法高效液相色谱法,采用ODS-50色谱柱,流动相为0.04M磷酸盐缓冲液(pH 11.0)-乙腈(400∶600),检测波长215 nm,柱温40℃,进样量20μL,溶出介质为磷酸盐缓冲液(pH6.5),转数为75 r/min,45 min取样。紫外分光光度法以磷酸盐缓冲液(pH6.0)为空白溶液及溶剂,检测波长为(482±2)nm,溶出介质为磷酸盐缓冲液(pH6.0),转速为100 r/min,45 min取样。结果溶出曲线方程式为:Y=0.001 3X+0.913,10 min时累计溶出量为92.3%(RSD=1.9%)。回归方程:A=0.007 5C-0.017 1,r=0.999 1。线性范围在17.9~89μg/mL,回收率为99.6%(RSD=0.4%)。结论两种方法都较为准确、简便,测得的溶出效果较好,溶出度结果也基本一致。     

HPLC assay of Lidocaine in plasma with solid phase extraction and UV detection

A sensitive and reliable method based on solid-phase extraction and reversed-phase liquid chromatography was developed and validated for the quantitation of Lidocaine (Lid) in dog plasma. Phenacemide was used as an internal standard (IS) in the extraction which employed C18 solid-phase extraction cartridges. The washing and eluting solutions were 2 ml acetonitrile-pH 9.0 phosphate buffer (10:90 v/v) and 0.5 ml acetonitrile-pH 4.0 phosphate buffer (40:60 v/v). respectively. The eluent obtained from the cartridge was directly analyzed on a reversed-phase ODS column with UV detection at 210 nm. A clean chromatogram and high sensitivity were achieved at this wavelength. The mobile phase was acetonitrile and pH 5.9 phosphate buffer (20:80 v/v). The retention times were 6.4 and 7.2 min for Lid and IS, respectively, at a flow rate of 1.0 ml min(-1). The mean absolute recovery was 96.6% (n = 9) with a CV of 3.8% for Lid and 81.7% with CV of 2.5% (n = 3) for IS. The limit of quantitation was 20 ng ml(-1), with the intra- and inter-day precisions (n = 5) of 4.4 and 3.4%, respectively, and the intra- and inter-day accuracies (n = 5) of -4.3 and -5.0%, respectively. For the analyses of Lid in spiked plasma samples at 20, 100 and 200 ng ml(-1), the overall mean intra- and inter-day precisions (n = 15) were 3.9 and 4.9%, respectively, and the overall mean intra- and inter-day accuracies (n = 15) were -3.7 and -4.6%, respectively. The correlation coefficients for calibration plots in the range 20-1000 ng ml(-1) in plasma were typically higher than 0.998. The suitability of the method was demonstrated by the study in a beagle dog receiving a low intravenous dose of Lid.     

Indirect polarographic and cathodic stripping voltammetric determination of cefaclor as an alkaline degradation product

Cefaclor is not reducible at a mercury electrode, but it can be determined polarographically and by cathodic stripping voltammetry as its initial alkaline degradation product which is obtained in high yield by hydrolysis of cefaclor in Britton-Robinson (B-R) buffer pH 10 at 50 degrees C for 30 min (reduction peak at pH 10, -0.70 V). Differential pulse polarographic calibration graphs are linear up to at least 1 x 10(-4) mol/l(-1). Recoveries of 93% of the cefaclor (n = 3) were obtained from urine spiked with 38.6 microg/ml(-1) using this polarographic method with 1 ml urine made up to 10 ml with pH 10 buffer. Using cathodic stripping voltammetry and accumulating at a hanging mercury drop electrode at - 0.2 V for 30 s, linear calibration graphs were obtained from 0.35 to 40 microg/ml(-1) cefaclor in B-R buffer pH 10. A relative standard deviation of 4.2% (eta = 5) was obtained, and the limit of detection was calculated to be 2.9 ng/ml(-1). Direct determination of cefaclor in human urine (1 ml of urine was made up to 10 ml with pH 10 buffer) spiked to 0.39 microg/ml(-1) was made (recovery 98.6%).     

RP-HPLC法测定蒲公英中绿原酸与咖啡酸的含量

目的测定蒲公英中绿原酸与咖啡酸的含量。方法采用Diamonsil C18色谱柱,流动相为乙腈-磷酸二氢钠缓冲液(13∶87,v/v),检测波长323 nm。结果绿原酸在2.4~48.0μg/mL(r=0.999 5),咖啡酸在1.0~20.0μg/mL(r=0.999 7)线性关系良好,咖啡酸、绿原酸的平均回收率分别为99.7%(RSD=0.8%)和100.8%(RSD=1.1%)。结论该方法准确、可靠、重现性好,可作为控制蒲公英药材质量的方法。     

乙醇摄入对盐酸苯环壬酯控释片释放行为的影响

目的：考察乙醇摄入对盐酸苯环壬酯控释片释放行为的影响。方法：测定盐酸苯环壬酯控释片中盐酸苯环壬酯原料在不同浓度乙醇磷酸盐缓冲液（pH3.0）中溶解度;关键辅料WSR-HM、WSR-LM在不同浓度乙醇磷酸盐缓冲液（pH3.0）中的黏度;以0%、5%、20%、30%、40%乙醇磷酸盐缓冲液（pH3.0）为释放介质,考察并比较盐酸苯环壬酯控释片的体外累积释放度,并采用扫描电镜观察释放介质中不同浓度的乙醇对盐酸苯环壬酯控释片薄膜衣的表面结构和释药孔的影响。据此分析乙醇影响盐酸苯环壬酯控释片体外释放的原因。结果：盐酸苯环壬酯在pH3.0磷酸盐缓冲液和5%、20%、30%、40%乙醇磷酸盐缓冲液（pH3.0）中的溶解度分别为39.6,47.3,84.7,171.4,235.4 mg·mL^-1;WSR-HM、WSR-LM的黏度随释放介质中乙醇浓度的增加而下降;盐酸苯环壬酯控释片在pH 3.0磷酸盐缓冲液和5%乙醇磷酸盐缓冲液释放介质中的释放曲线相似（相似因子f₂=74）,但在20%、30%、40%乙醇磷酸盐缓冲液（pH3.0）释放介质中的释放度有显著变化;盐酸苯环壬酯控释片完全释放后,残留释药孔的直径分别为552,600,630,718,815 μm。结论：5%乙醇对盐酸苯环壬酯控释片的释放影响最小,而随着乙醇浓度的增加,乙醇通过改变盐酸苯环壬酯溶解度、WSR-HM及WSR-LM黏度和溶胀程度从而对盐酸苯环壬酯控释片的释放产生影响,并且乙醇浓度越大,体外释放越快。     

Chiral separation of cefadroxil by capillary electrochromatography

In this paper, the chiral separation of cefadroxil was studied by capillary electrochromatography. Monolithic capillary column was prepared for the separation of cefadroxil enantiomers. The optimum buffer contained 28.5 mmol/L sodium acetate, 0.95% (v/v) acetic acid, 19 mmol/L beta-cyclodextrin (beta-CD) and 5% (v/v) isopropanol in formamide solution (pH 7.0), with the running voltage of 12 kV, the UV detector wavelength of 254 nm, the sample injected time of 8s and the temperature of 25 degrees C. Under these conditions, the column efficiency of cefadroxil enantiomers were N1=5324 and N2=23,768 with a selectivity factor (alpha) of 1.056 and resolution (Rs) of 0.978. The effect of buffer pH value, beta-CD concentration, organic modifier (isopropanol) concentration and voltage was also investigated for the separation by CEC.     

高效液相色谱法测定复方磺胺甲噁唑混悬剂的含量

目的　采用HPLC法测定复方磺胺甲唑混悬剂中磺胺甲唑 (SMZ)和甲氧苄啶 (TMP)的含量。方法　采用Zor baxSB C18色谱柱 ;以磷酸盐缓冲液 乙腈 (75∶2 5)为流动相 ;流量为 1 0ml/min ;检测波长为 2 3 0nm ;用外标法测定。结果　平均回收率 :SMZ为 99 68% ,RSD为 0 2 6% ;TMP为 10 0 6% ,RSD为 0 76%。结论　该方法简便、准确、可靠 ,适用于复方磺胺甲唑混悬剂的定量检测。     

黄芩苷在不同pH值缓冲液中理化常数的测定

目的考察黄芩苷在不同pH值中的平衡溶解度与表观油水分配系数,为制剂研究奠定基础。方法采用摇瓶-紫外分光光度法测定温度为25和37℃时,黄芩苷在不同pH值磷酸盐缓冲溶液中的平衡溶解度及在正辛醇/缓冲液体系中的表观油水分配系数。结果 25℃时,黄芩苷在pH=2.0,3.0,4.0,5.0,6.0,6.8,7.4,8.0和9.0缓冲液中的平衡溶解度分别为0.032,0.034,0.119,0.873,3.329,12.96,11.49,4.605和11.87mg.mL-1,相应条件下表观油水分配系数(P)值分别为0.363,0.244,0.292,0.137,0.057,0.046,0.036,0.028和0.029。37℃时,黄芩苷在pH=2.0,3.0,4.0,5.0,6.0,6.8,7.4,8.0和9.0缓冲液中的平衡溶解度分别为0.028,0.048,0.095,0.950,4.881,14.15,26.65,14.48和17.89mg.mL-1,相应条件下表观油水分配系数(P)值分别为0.234,0.224,0.365,0.103,0.074,0.049,0.034,0.034和0.035。结论黄芩苷的平衡溶解度在酸性及中性条件下受温度影响很小,在碱性条件下随着温度升高而增加;黄芩苷在酸性条件下的P值比在碱性条件下大,Pmax=0.363(T=25℃,pH=2),Pmax=0.365(T=37℃,pH=4),随着碱性的增加P值变化不明显,且温度对黄芩苷的P值几乎无影响。