高效液相色谱法测定复方利多卡因乳膏中丙胺卡因与利多卡因的含量

目的：探讨复方利多卡因乳膏质量控制方法，为该药的质量控制提供依据。方法：采用高效液相色谱法。结果：丙胺卡因在133－240mg.L^-1，利多卡因在140－250mg.L^-1范围内呈现良好的线性关系，r均为0．9996，样品回收率高，丙胺卡因和利多卡因回收率分别为99．27％和99．05％，RSD分别为1．14％和0．67％，样品溶液稳定，3d内日间差异性试验结果：丙胺卡因RSD＝0．73％，利多卡因RSD＝0．65％，本实验方法重复性好，RSD分别为丙胺卡因1．30％，利多卡因0．91，对3批样品进行含量测定，结果分别为：丙胺卡因99．69％，100．53％，101．86％，利多卡因99．67％，98．30％，99．97％，结论：本方法准确，可靠，能同时测定复方利多卡因乳膏中利多卡因，丙胺卡因的含量，在本研究基础上制定的质量标准可以控制本品的质量，方法具有可行性。     

高效液相色谱法同时测定双氯芬酸钠和利多卡因的含量

目的：测定复方双氯芬酸钠注射液中双氯芬酸钠和利多卡因的含量。方法：采用高效液相色谱法，Kromasil-C18为色谱柱，4．1％醋酸钠溶液（pH5.5)－甲醇（30：70）为流动相；检测波长为220nm，柱温25℃。结果：双氯芬酸钠性范围为29．95－299．52mg.L^-1，平均回收率为99．29％（RSD为0．77％,n=9）；利多卡因线性范围为6．85－68．52mg.L^-1，平均回收率为101．3％（RSD为0．76％，n=9)。结论：该法简便，灵敏，准确。     

HPLC法测定血浆及尿液中左氧氟沙星的浓度

采用高效液相色谱－荧光法测定了血浆及尿液中左氧氟沙星的浓度。Nova－PakC18预柱，SymmetryC18分析柱，已腈－0．05mol/L枸橼酸－1mol/L醋酸铵（11．5：77：1）为流动相，激发波长300um，发射波长500um。血中左氧氟沙星回收率为100．5％，RSD为1％。尿中左氧氟沙星回收率为99．0％，RSD为1．6％。最低检测量为8ng。     

高果糖浆中果糖和葡萄糖的HPLC测定

建立了高果糖浆中果糖和葡萄糖含量测定的HPLC法。采用Kromasil KR100-5 NH2柱，乙腈－水（77．5：22．5）为流动相，流速1．0ml/min，差示折光检测，外标法测定。果糖与葡萄糖在0．1－10mg/ml的浓度范围内均线性良好，r分别为0．9999和0．9997；果糖和葡萄糖的日内、日间精密度RSD小于2．0％；平均回收率分别为99．5％（RSD1．2％0和99．6％（RSD1．0％）。     

碳酸利多卡因注射液含量测定方法的改进

目的：建立碳酸利多卡因注射液中碳酸利多卡因的含量测定方法。方法：采用HPLC法测定,色谱柱为DiamonsilC18柱;流动相为乙腈．pH8．0磷酸盐缓冲液（印：40）,流速为1．0mL·min^-1,检测波长为254nm。结果：利多卡因线性范围为1．7552～15．7968μg;平均回收率（n=9）为99．04％（RSD％为0．17％）。结论：方法简便、快速,专属性强,可有效的控制碳酸利多卡因注射液中利多卡因的含量。     

高效毛细管电泳法测定注射用哌拉西林／三唑巴坦的含量

建立注射用哌拉西林／三唑巴坦的HPCE含量测定方法。方法：测定条件为：运行缓冲液：25mmol/L的磷酸硼砂溶液和50mmol/L的SDS，pH9.0；操作电压20kV，检测波长200nm。结果：测定哌拉西林的线性范围为0．01－0．75mg/ml,日内RSD为0．66％，日间RSD为0．88％；三唑巴坦的线性范围为0．02－1．0mg/ml,日内RSD为0．71％，日间RSD为0．98％。哌拉西林的回收率为99．76％，三唑巴坦的回收率为98．2％。结论：该方法简便、经济、快速，准确可靠。     

复方福尔可定口服液的HPLC和TLC测定

建立了HPLC法和TLC法分别测定复方福尔可定口服液的含量和有关物质。HPLC采用AlltimaC18色普柱，流动相对为甲醇－1．0％十二烷基硫酸钠溶液－冰醋酸25：55：35：0．3），检测波长为265nm，3个主成分的平均回收率分别为99．5％（RSD0．71％）、100．0％（RSD0．305）和100．0％（RSD0．85％）。线性相关系数均大于0．9992，日内、日间精密度均小于0．60％。TLC以硅胶G薄层层析板，展开剂为乙醇－甲苯－丙酮－浓氨溶液（70：70：65：5）。     

HPLC法同时测定复方水杨酸搽剂中三组分的含量

目的：建立高效液相色谱法同时测定复方水杨酸搽剂中3组分含量的方法。方法：采用Hypersil BDS C18（4．6mm×200mm，5μm）色谱柱，0．1mol·L^-1磷酸氢二钠溶液-甲醇（60：40，用20％磷酸调节pH5．0）为流动相，流速为1．0mL·min^-1，检测波长为212nm。结果：间苯二酚、水杨酸、苯酚分别在0．0388—0．776μg（r=0．9999），0．1176～2．352μg（r=0．9999）、0．0218～0．436μg（r=0．9999）范围内线性关系良好，3个浓度组间苯二酚的平均回收率分别为99．0％（RSD=0．3％），97．2％（RSD=0．5％），98．5％（RSD=0．8％），水杨酸的平均回收率分别为100．3％（RSD=0．4％），99．5％（RSD=0．7％），97．5％（RSD=0．6％），苯酚的平均回收率分别为97．1％（RSD=1．1％），97．8％（RSD=0．7％），99．6％（RSD=0．9％）。结论：本测定方法简便、快速、准确，为复方水杨酸搽剂质量评价提供了可靠方法。     

利多卡因羟甲唑啉溶液的质量标准研究

目的：建立利多卡因羟甲唑啉溶液的质量标准。方法采用化学显色法和色谱法对利多卡因和羟甲唑啉进行鉴别，并用高效液相色谱法分别测定利多卡因和羟甲唑啉的含量。结果制剂为无色至微黄色液体，鉴别、检查项均符合2010年版《中国药典》中的相关规定；利多卡因和羟甲唑啉分别在4．006～20．03μg （ r＝0．9994）和0．1004～0．5002μg （ r＝0．9990）范围内线性关系良好，二者的平均回收率分别为100．4％（RSD＝1．0％）和99．2％（RSD＝1．2％）。结论所建立的标准可用于该制剂的质量控制。     

复方环麻滴鼻凝胶剂的制备及质量控制

目的：制备复方环麻滴鼻凝胶剂有其质量控制。方法：以卡波姆－940为乳化剂，三乙醇胺调节pH,制备水溶性透明凝胶。用紫外分光光工法和旋光度分别测定凝胶剂中盐酸丙沙星和盐酸麻黄碱的含量。结果：制备的凝胶均匀细腻，稠度适宜。盐酸环丙沙星的含量平均值为102．3％，RSD为1．86％；平均回收率为99．4％，RSD为0．26％。盐酸麻黄碱的平均含量为103．7％，RSD为2．8％；平均回收率为99．7％，RSD为0．81％。结论：该制剂性能稳定，无刺激性，测定方法简单易行，快速准确，适合医院制剂。     

高效液相色谱法测定曲美胶囊中盐酸西布曲明的含量

目的:建立测定曲美中盐酸西布曲明含量的高效液相色谱法。方法:分析柱为Diamonsil C18(250mm×4.6mm,5μm),流动相为甲醇-水-三乙胺(75:25:0.1),检测波长为223nm,流速为1.0ml/min。结果:盐酸西布曲明在0.0 106～0.2 110mg/ml范围内呈良好线性关系,平均回收率为100.3%,RSD=0.81％。结论:本法检测快速,定量准确,可用于曲美中盐酸西布曲明含量测定。     

高效液相色谱法测定人血浆中盐酸美沙酮浓度

目的:测定人血浆中盐酸美沙酮的含量。方法:采用高效液相色谱法(HPLC)。色谱条件:Symmetry-C_(18)柱,流动相:乙腈-磷酸二氢钾(38:62,v/v),检测波长220nm。结果:本法在0.02-1μg·ml~(-1)的范围内线性良好,r=O.9999。日内、日间的相对标准偏差RSD<1.5％,平均回收率为98.97％。结论:本法简便、快速、准确。     

超快速液相色谱法测定新型“K2”香料中JWH-018的含量

目的:建立测定新型"K2"香料中JWH-018含量的超快速液相色谱法。方法:采用Shim-pack XR-ODSⅡ色谱柱(2.0 mm×75 mm,2.2μm);流动相:乙腈(含0.1%甲酸)-水(含0.1%甲酸)(80:20,v/v),流速:0.25 mL·min-1;检测波长280 nm,柱温:35℃,进样量:2μL,外标法定量测定JWH-018的含量。结果:JWH-018的浓度在1-1000μg·mL-1范围内线性良好(A=8419.8C+13932,r=1.0000);最低检测限为90 ng·mL-1(S/N=3);低、中、高3种浓度的加样回收率(n=3)分别为101.0%(RSD=0.28%),101.0%(RSD=0.63%),101.7%(RSD=0.03%)。结论:本法操作简便、灵敏、准确,重复性好,适用于"K2"香料中JWH-018含量的测定。     

Validated high performance liquid chromatographic method for simultaneous determination of phenytoin, phenobarbital and carbamazepine in human serum

A high performance liquid chromatographic (HPLC) method for the simultaneous determination of phenytoin (CAS 57-41-0), phenobarbital (CAS 50-06-6, phenobarbitone) and carbamazepine (CAS 298-46-4) is described. The serum was extracted with ethyl acetate, the dried extract was reconstituted in mobile phase and the aliquot was injected. The eluent drugs were detected at 230 nm. The mobile phase consisting of methanol: water: glacial acetic acid mixture (67:33:1, v/v/v) was used at a flow rate of 1 ml/min on C-18 column. The absolute recovery was above 96% of all the three drugs over a concentration range of 0.5-50.0 micrograms/ml. The inter-day and intra-day precision relative standard deviation (RSD) ranged from 0.79-5.13% and 0.11-6.81%, respectively. The method is simple, rapid, accurate and sensitive and is presently used for therapeutic drug monitoring in epileptic patients. The results obtained with this method showed very good clinical correlation.     

Stability-indicating HPLC method for posaconazole bulk assay

A stability-indicating liquid chromatographic (LC) method was developed for the determination of posaconazole in bulk. Chromatographic separation was achieved using an isocratic elution in a reversed-phase system, with a mobile phase composed of methanol-water (75:25, v/v), at 1.0 mL min(-1) flow. Samples were exposed to degradation under thermal, oxidative and acid/basic conditions, and no interference in the analysis was observed. System suitability was evaluated and results were satisfactory (N = 4,900.00 tailing factor 1.04; RSD between injections = 0.65). The retention time of posaconazole was about 8.5 min and the method was validated within the concentration range 5-60 μg mL(-1) (r = 0.9996). Adequate results were obtained for repeatability (RSD % = 0.86-1.22), inter-day precision (RSD % = 1.21) and accuracy (98.13% mean recovery). Robustness was also determined to be satisfactory after evaluation. The proposed method was successfully applied to posaconazole bulk quantification, showing the method is useful for determination of the drug in routine analysis.     

Validated HPLC method for determination of PAT-5A, an insulin sensitizing agent, in rat plasma

A high performance liquid chromatographic method for the determination of PAT-5A (a potent insulin sensitizer) using DRF-2095 (a thiazolidinedione) as internal standard (I.S.) is described. A 1:1 v/v ethylacetate and dichloromethane solvent mixture was used for extraction of PAT-5A from plasma. A Kromasil KR100-5C18-250A, 5 microm, 4.6 x 250 mm SS column was used for the analysis. Mobile phase consisting of sodium dihydrogen phosphate (pH 4.0, 0.05 M) and methanol mixture (25:75, v/v) was used at a flow rate of 1.0 ml/min. The eluate was monitored using a UV detector set at 345 nm. Ratio of peak area of analyte to I.S. was used for quantification of plasma samples. Using this method the absolute recovery of PAT-5A from rat plasma was > 90% and the limit of quantification was 0.05 microg/ml. The intra-day relative standard deviation (RSD) ranged from 2.19 to 4.98% at 1.0 microg/ml, 1.05 to 3.68% at 10.0 microg/ml and 3.14 to 5.08% at 50 microg/ml. The inter-day RSD were 1.6, 2.24 and 1.54% at 1, 10 and 50 microg/ml, respectively. The method was applied to measure the plasma concentrations of PAT-5A in pharmacokinetic and bioavailability studies in male Wistar rats.     

RSD1019 suppresses ischaemia-induced monophasic action potential shortening and arrhythmias in anaesthetized rabbits

The electrophysiological actions of lidocaine, tedisamil and RSD1019 were assessed on normal and ischaemic cardiac tissue using monophasic action potentials (MAPs) recorded from the epicardium of anaesthetized rabbits. Drug effects on ischaemia-induced arrhythmias were assessed simultaneously in the same rabbits. Lidocaine, infused at 2.5, 5 and 10 micromol kg(-1) min(-1) i.v., accelerated and worsened the electrophysiological derangement caused by ischaemia, had profibrillatory actions and reduced the time to the occurrence of ventricular fibrillation (VF) relative to controls. Tedisamil, infused at 0.063, 0.125 and 0.25 micromol kg(-1) min(-1) i.v., prolonged MAP duration at 90% repolarization (MAPD(90%)) before induction of ischaemia in a dose-related manner; however, this effect was not maintained 5 min after induction of ischaemia. Tedisamil had no significant antiarrhythmic actions over the dose-range tested. RSD1019, infused at 2, 4 and 8 micromol kg(-1) min(-1) i.v., produced a small increase in MAPD(90%) before induction of ischaemia and only at the highest dose tested. In contrast to tedisamil, RSD1019 suppressed ischaemia-induced MAP shortening assessed 5 min after induction of ischaemia. This effect was dose-related. RSD1019 completely prevented ischaemia-induced tachyarrhythmias at the mid and highest infusion levels tested. The results of this study illustrate a pathologically targeted approach for preventing ischaemia-induced arrhythmias. Suppression of ischaemia-induced MAP shortening, demonstrated herein for RSD1019, represents a novel antifibrillatory approach.     

HPLC法测定复方克霉唑乳膏中二苯基-(2-氯苯基)甲醇和克霉唑的含量

目的：建立HPLC法测定复方克霉唑乳膏中二苯基-（2-氯苯基）甲醇和克霉唑的含量。方法：采用WatersC18色谱柱,以0．05mol·L-1的磷酸二氢钾溶液-甲醇（3：7）,用10％磷酸调pH至5．7～5．8为流动相,检测波长215nln,流速1．5mL·min-1,柱温30℃。结果：二苯基-（2-氯苯基）甲醇和克霉唑分别在5．096×10-3 0．2038μg（r=0．9999）和0．1062～1．062μg（r=0．9999）范围线性关系良好,平均加样回收率分别为99．15％和100．69％（RSD分别为0．79％和0．66％）。结论：本法简便、准确、精密度高,可用于复方克霉唑乳膏的质量控制。     

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。