苯酰甲硝唑分散片的血药浓度及生物等效性测定

目的:建立人血清中苯酰甲硝唑体内代谢产物--甲硝唑的反相高效液相色谱分析方法,比较苯酰甲硝唑分散片和苯酰甲硝唑胶囊生物等效性。方法:采用Eurosphex-100 C18柱,以乙腈-KH2PO4(0．01 mol·L-1)(22:78,v／v)为流动相,替硝唑作内标,紫外检测波长为318 nm,测定血清中甲硝唑的血药浓度。结果:血清中甲硝唑的浓度在0．1-20．0μg·ml-1范围内线性关系良好,r=0．999 9(n=8)。受试制剂及参比制剂的Cmax分别为(10．475±2．135)和(10．118±2．116),Tmax分别为(4．000±1．414)和(4．667±1．138)h,t1／2分别为(11．247±2．264)和(10．800±2．000)h,根据AUC0→t计算受试制剂的相对生物利用度为(100．9±20．2)％。结论:本方法操作简便、灵敏度高、重现性好,可用于血清中甲硝唑浓度的测定。苯酰甲硝唑分散片和苯酰甲硝唑胶囊具有生物等效性。     

反相高效液相色谱法测定苯酰甲硝唑有关物质

目的:建立反相高效液相色谱法测定苯酰甲硝唑有关物质。方法:采用双波长检测,梯度洗脱。色谱柱为迪马公司 Dia-monsil~(TM)C_(18)(250mm×4.6mm,5μm);流动相 A 和 B 分别为1.5g·L~(-1)磷酸二氢钾溶液(用1mol·L~(-1)磷酸溶液调 pH3.2)-乙腈(80:20和58:42);流速1.0mL·min~(-1),检测波长为235,315nm,进样量20μL,柱温为室温,外标法和主成分自身对照法计算。结果:杂质 A、杂质 B、杂质 C、苯酰甲硝唑均能达到很好的分离,并分别在1.12～16.8μg·mL~(-1)(r=1.000),1.12～16.8μg·mL~(-1)(r=0.9999),1.0～15.0μg·mL~(-1)(r=1.000),1.04～15.6μg·mL~(-1)(r=0.9992)浓度范围内具有良好的线性关系。杂质 A、杂质 B、杂质 C 的平均回收率(n=9)分别为99.4%,99.6%,99.5%。结论:本法简便、灵敏、准确,专属性强,适合于苯酰甲硝唑有关物质的测定。     

离子对-反相高效液相色谱法测定布洛伪麻分散片的含量

目的:建立布洛伪麻分散片含量的测定方法.方法:色谱柱为Kromasil C18柱(4.6 mm×150 mm,5 μm),流动相为醋酸-醋酸钠缓冲液:乙腈(4:6),每1 000 mL流动相溶解十二烷基硫酸钠1.0 g;检测波长为257 nm.结果:布洛芬和盐酸伪麻黄碱含量测定的线性范围分别为0.8～8 mg/mL(r=0.999 8)和0.12～1.2 mg/mL(r=0.999 9),平均回收率分别为101.7%(RSD=0.53%,n=9)和100.2%(RSD=0.8%,n=9).结论:该方法简便、重现性好,适用于布洛伪麻分散片的质量控制.     

高效液相色谱法测定苯酰甲硝唑胶囊含量

目的：建立HPLC法测定苯酰甲硝唑胶囊中苯酰甲硝唑含量的方法。方法：色谱柱为Shimpack CLC—ODS柱（4．6mm×150mm,5μm）;流动相乙腈-KH2P04（0．01mol/L）（22：78）,流速1．0ml／min;柱温室温;检测波长310nm。结果：苯酰甲硝唑与处方敷料分离良好,线性范围为4—40μg／ml（r=0．9998,n=5）,平均回收率96．6％,RSD为0．71％。结论：该法简便可靠,可用于苯酰甲硝唑胶囊的含量测定。     

中药直肠滴入治疗慢性盆腔炎的效果分析

目的探讨中药直肠滴入治疗慢性盆腔炎的临床效果。方法将我院2011年1月至2013年1月收治的慢性盆腔炎患者200例随机分为观察组100例(中药直肠滴入)和对照组100例(口服苯酰甲硝唑分散片),对两组治疗效果进行对比分析。结果观察组总有效率为95%(95/100),对照组总有效率为77%(77/100),两组相比差异具有显著性(P<0.05)。结论中药直肠滴入治疗慢性盆腔炎方便,安全,疗效显著,值得在临床上大力推广使用。     

HPLC法同时测定复方甲硝唑克林霉素乳膏中4种成分的含量

目的:建立同时测定复方甲硝唑克林霉素乳膏中甲硝唑、盐酸克林霉素、螺内酯、维生素B_6含量的方法。方法:采用高效液相色谱法。色谱柱为Diamonsil C_(18),流动相为乙腈-[0.68%磷酸氢二钾溶液(含1%三乙胺)](梯度洗脱),流速为1.0 mL/min,检测波长为210 nm,柱温为25℃,进样量为20μL。结果:甲硝唑、盐酸克林霉素、螺内酯、维生素B_6检测质量浓度线性范围分别为20.0～120.0μg/mL(r=0.999 9)、10.0～60.0μg/mL(r=0.999 1)、4.0～24.0μg/mL(r=0.999 4)、10.0～60.0μg/mL(r=0.999 4);定量限分别为13.06、7.36、2.43、6.42μg/mL,检测限分别为4.18、1.82、0.76、1.79μg/mL;精密度、稳定性、重复性试验的RSD<2.0%;回收率分别为98.97%～100.91%(RSD=0.79%,n=9)、99.02%～101.80%(RSD=1.03%,n=9)、98.18%～101.05%(RSD=1.01%,n=9)、98.75%～101.36%(RSD=0.87%,n=9)。结论:该方法简便、快速、结果准确,可用于复方甲硝唑克林霉素乳膏中甲硝唑、盐酸克林霉素、螺内酯、维生素B_6含量的同时测定。     

HPLC法测定甲硝唑结肠定位肠溶胶囊含量

目的:研究HPLC法测定甲硝唑结肠定位肠溶胶囊含量。方法:采用C 18分析柱,甲醇-乙腈-磷酸二氢钾(20∶20∶60)为流动相,流速1.0 mL/m in,检测波长317 nm。结果:甲硝唑在4.02~24.12μg/mL范围内呈良好线性关系(r=0.9998),平均回收率为99.2%(RSD 0.64%)。结论:本方法实用、快速,适用于临床医院的药检。     

高效液相色谱法测定氯霉素甲硝唑搽剂的含量

目的建立高效液相色谱法同时测定氯霉素甲硝唑搽剂中两组分含量。方法采用高效液相色谱法测定氯霉素和甲硝唑的含量。色谱条件为:Agilent Extend-C18色谱柱(4.6×250mm),流动相:甲醇-水-冰醋酸(45∶55∶0.1),流速1.0mL/m in,检测波长280nm,柱温30℃,进样量10μL。结果线性范围分别是:氯霉素49.82μg/mL~498.20μg/mL,r=0.9999;甲硝唑39.74μg/mL~397.40μg/mL,r=0.9999;平均回收率±RSD分别为99.42%±0.97%,99.83%±0.70%。结论本法简便,快速,准确,适用于该制剂中氯霉素和甲硝唑含量测定。     

梯度高效液相色谱法测定苯酰甲硝唑原料药的有关物质

目的:建立梯度高效液相色谱法测定苯酰甲硝唑有关物质的方法。方法:采用梯度洗脱方法。色谱柱为Phen-omsil C18(250mm×4.6mm,5μm);流动相A为磷酸盐缓冲液(取磷酸二氢钾1.5g,加水溶解并稀释至1 000mL,用磷酸调节pH至3.2),流动相B为乙腈,以0.9mL.min-1流速进行梯度洗脱,梯度洗脱条件:0~5min,A为76%;5~15min,A从76%→65%;15~60min,A为65%;60~60.1min,A从65%→76%;60.1~75min,A为76%;检测波长为232nm;柱温40℃;进样量10μL。照杂质对照品对照法和不加校正因子的主成分自身对照法检查。结果:杂质2-甲基-5-硝基咪唑、甲硝唑、苯甲酸均能达到很好的分离,并分别在0.2516~5.032mg.L-1(r=0.999 9),0.2456~4.912mg.L-1(r=1.000 0),0.066 8~1.336mg.L-1(r=0.999 9)范围内具有良好的线性关系。2-甲基-5-硝基咪唑、甲硝唑、苯甲酸的平均回收率(n=9)分别为97.93%(RSD为1.03%),97.63%(RSD为0.46%),...     

高效液相色谱法测定甲硝唑漱口液中甲硝唑含量

目的建立测定甲硝唑漱口液中甲硝唑含量的高效液相色谱法。方法采用Ultimate C18色谱柱(250 mm×4.6 mm,5μm),以甲醇-0.075 mol/L磷酸二氢钾溶液(13∶87)为流动相,流速为1.0 mL/min,检测波长为274 nm。结果甲硝唑质量浓度在50～200μg/mL范围内与峰面积线性关系良好(r=1.000 0,n=5),平均回收率为99.19%,RSD=0.53%(n=6)。结论该方法简便、快速、准确,可用于甲硝唑漱口液的甲硝唑含量测定。     

高效液相色谱法测定更年宁心片中盐酸小檗碱的含量

目的建立测定更年宁心片中盐酸小檗碱含量的高效液相色谱法。方法以十八烷基硅烷键合硅胶为填充剂;以乙腈-水(每100mL加0.26mL磷酸、0.5mL三乙胺与0.05g十二烷基硫酸钠)(46:54)为流动相;检测波长为264nm。结果盐酸小檗碱在8.02～72.18μg/mL范围内线性关系良好,平均回收率为100.19%,RSD为1.21%(n=5)。结论该方法稳定,重现性好,可作为更年宁心片中盐酸小檗碱的含量测定方法。     

反相高效液相色谱法测定吡罗昔康胶囊中吡罗昔康含量

目的建立测定吡罗昔康胶囊中吡罗昔康含量的反相高效液相色谱法。方法色谱柱为Kromasil C18柱（250mm×4.6mm,5μm）,流动相为磷酸二氢钾溶液（1.36g磷酸二氢钾,加水750mL,振摇使溶解,加1.7%浓磷酸溶液116mL,加水至1000mL）-甲醇（45：55）,流速1.0mL/min,检测波长361nm。结果吡罗昔康对照品溶液质量浓度在19.712～118.272μg/mL范围内与峰面积线性关系良好,r=0.9999,平均回收率为98.64%,RSD为0.42%（n=6）。结论所用方法快速、简便、准确、重现性好。     

高效液相色谱法测定头孢曲松钠中2-巯基苯并噻唑含量

摘要：目的 建立测定头孢曲松钠中基因毒性杂质2-巯基苯并噻唑含量的反相高效液相色谱法。方法 采用十八烷基硅 烷键合硅胶为填充剂(Agilent ZORBAX SB-Aq C18,4.6 mm×250 mm,5 μm)的色谱柱,流动相为1%甲酸溶液-乙腈(60:40, V/V),流速0.5 mL/min,检测波长320 nm,柱温25℃。结果 定量限为0.5 ppm(相当于样品浓度的百分比为0.00005%),检测 限为0.15 ppm。2-巯基苯并噻唑在0.0051~0.2051 μg/mL浓度范围内,线性方程为y=6.4195x-0.0098,r=0.9996＞0.999。回收率为 86.3%~102.3%(RSD＜10.0%,n=9)。结论 该方法操作简便、专属性强、灵敏度高,可有效检出头孢曲松钠中2-巯基苯并噻唑 的含量。     

Simultaneous determination of dextromethorphan and dextrophan in rat plasma by LC-MS/MS and its application to a pharmacokinetic study

A highly selective and sensitive liquid chromatography-tandem mass spectrometric (LC-MS/MS) method was developed and validated for quantitating dextromethorphan (DXM) and its metabolite dextrophan (DXO) in rat plasma using pirfenidone as an internal standard. Protein precipitation with acetonitrile was employed for the sample preparation. Chromatographic separation was achieved on a SB-C18 column at 25 degrees C, with a gradient elution programme of which acetonitrile-0.1% formic acid in water as mobile phase. The flow rate was 0.4 mL/min. Detection is carried out by multiple reaction monitoring (MRM) on a ion-trap LC-MS/MS system with an electrospray ionization interface. The assay is linear over the range 1-500 ng/mL for DXM and 1-250 ng/mL for DXO, with a lower limit of quantitation of 1 ng/mL for both. Intra- and inter-day precision of the assay were less than 9.80% and the accuracy were in the range 96.35-106.39%. The developed method was successfully applied to analyze the drug in samples of rat plasma for pharmacokinetic study.     

Determination of pinostrobin in rat plasma by LC-MS/MS: application to pharmacokinetics

A rapid and sensitive method for the determination of pinostrobin in rat plasma was developed using liquid chromatography tandem mass spectrometry (LC-MS/MS) for the first time. Isoliquiritigenin was used as an internal standard in rat plasma. Chromatographic separation was performed on an HiQ Sil C₁₈ column with isocratic elution at a flow rate of 1 mL/min. The mobile phase consisted of water and methanol (9:91, v/v) containing 0.1% formic acid. The quantification limit was 10 ng/mL within a linear range of 10-1000 ng/mL (R = 0.9984). The intra- and inter-day assay precision ranged from 3.8-5.3% to 3.2-5.2%, respectively, and the intra- and inter-day assay accuracy was between 93.2-95.1% and 95.5-104.3%, respectively. Our results indicated that the LC-MS/MS method is effective for pharmacokinetic study of pinostrobin in rat plasma.     

Toxicological analysis of chlorhexidine in human serum using HPLC on a polymer-coated ODS column

A simple and reliable high-performance liquid chromatographic (HPLC) method for analyzing chlorhexidine in human serum was developed. After the addition of an internal standard, levomepromazine, 0.2 mL serum was deproteinized with 10% perchloric acid. The acidic supernatant was neutralized with 1M potassium carbonate solution, and the insoluble salt was removed by centrifugation. An aliquot of the supernatant was applied to HPLC with UV detection (260 nm). HPLC separation was achieved on a polymer-coated ODS column equilibrated with acetonitrile/water containing 0.05% trifluoroacetic acid, 0.05% heptafluorobutyric acid, and 0.1% triethylamine (40:60, v/v). The calibration curve was linear in the concentration range from 0.05 to 50.0 microg/mL, and the lower limit of detection was 0.05 microg/mL. The accuracy and precision of the method were evaluated at concentrations of 0.5 microg/mL and 5.0 microg/mL. The coefficients of variation ranged from 4.0 to 4.5%. The concentration of chlorhexidine in the serum of a patient who died after a suspected intravenous injection of chlorhexidine gluconate was determined.     

高效液相色谱法测定膦甲酸钠滴眼液含量

目的建立高效液相色谱法测定膦甲酸钠滴眼液的含量。方法采用Diamonsil C18色谱柱（4.6 mm×200 mm,5μm）,流动相：A液-B液-四己基硫酸氢铵-甲醇（700∶300∶0.25∶100）（pH 4.4）（A液：硫酸钠3.22 g,冰醋酸3 mL,44.61 g.L-1焦磷酸钠6 mL,加水至1 000 mL;B液：硫酸钠3.22 g,醋酸钠6.8 g,44.61 g.L-1焦磷酸钠6 mL,加水至1 000 mL）,检测波长：230 nm,流速：1.0 mL.min-1,柱温：室温。结果膦甲酸钠在25.1~803.2μg.mL-1与峰面积呈良好的线性关系（r=0.999 9）,平均回收率100.1%,RSD=0.62%（n=9）。结论该方法简便、快速、准确、重复性好,可作为膦甲酸钠滴眼液的质量控制方法。     

Solid-phase microextraction for the assay of levomepromazine in human plasma

Solid-phase microextraction (SPME) was investigated as sample preparation for the assay of the neuroleptic drug levomepromazine in human plasma. A mixture of human plasma, water, chloramitriptyline as internal standard, and aqueous NaOH was extracted with a 100-microm polydimethylsiloxane (PDMS) fiber (Supelco). The desorption of the fiber was performed in the injection port of a gas chromatograph at 260 degrees C [HP 5890; BPX-5 (SGE): 30 m x 0.53 mm ID, 1-microm film capillary; nitrogen-phosphorus selective detection]. As repeatedly found for SPME analysis of drugs in plasma, the recovery was low (i.e., 7% for levomepromazine). However, the analyte and internal standard were well separated and the calibration was linear from 5 to 180 ng/mL. The within-day precision was 2%, 4%, and 19% at concentrations of 160 ng/mL, 80 ng/mL, and 5 ng/mL, respectively. The between-day precision was 3%, 7%, and 19%, respectively. The limit of determination was 5 ng/mL. The comparison with an established liquid-liquid extraction gas-liquid chromatography method revealed good agreement for spiked samples and patient samples. No interfering peaks of drugs coadministered with levomepromazine or of endogenous substances were found. It is concluded that the method can be used in the therapeutic drug monitoring and clinical toxicology of levomepromazine.     

芹菜素固体脂质纳米粒处方前的研究

目的建立HPLC法测定固体脂质纳米粒中芹菜素的含量,并对其进行处方前研究。方法色谱柱:KromasilODS柱(200mm×4.6mm,5μm);流动相:乙腈:水(55:45,v/v);流速:1.0mL/min;检测波长:340nm。用HPLC法测定芹菜素在制备温度下溶液中的稳定性、水中溶解度以及表观油/水分配系数。结果芹菜素的线性范围:1.00～32.00μg/mL,r=1,平均回收率:100.93。芹菜素75℃下稳定性良好,水中溶解度为2.34μg/mL,表观油/水分配系数P=3.23。结论本法准确、快速、重现性好,适合芹菜素固体脂质纳米粒的体外含量测定。可根据芹菜素的理化性质,将其制备成固体脂质纳米粒。     

Determination of capsaicin,nonivamide, and dihydrocapsaicin in blood and tissue by liquid chromatography-tandem mass spectrometry

A sensitive and selective liquid chromatography-tandem mass spectrometry (LC-MS-MS) method for the analysis of capsaicin, nonivamide, and dihydrocapsaicin in blood and tissue has been developed. The method utilized a one-step liquid-liquid extraction that yielded an approximate 90% recovery of capsaicinoids from blood. Chomatographic separation of the capsaicinoids was achieved using a reversed-phase high-performance liquid chromatography column and a stepwise gradient of methanol and distilled water containing 0.1% (v/v) formic acid. Identification and quantitation of the capsaicinoids was achieved using electrospray ionization-tandem mass spectrometry monitoring the precursor-to-product-ion transitions for the internal standard octanoyl vanillamide (m/z 280 --> 137), capsaicin (m/z 306 --> 137), dihydrocapsaicin (m/z 308 -->137), and nonivamide (m/z 294 --> 137). Calibration curves, 1.0 to 250 ng/mL, were constructed by plotting concentration versus peak-area ratio (analyte/internal standard) and fitting the data with a weighted quadratic equation. The accuracy of the assay ranged from 90% to 107% for all analytes. The intra-assay precision (%RSD) for capsaicin was 4% at 2.5 ng/mL, 3% at 10 ng/mL, and 7% at 100 ng/mL. The interassay precision (% RSD) for capsaicin was 6% at 2.5 ng/mL, 6% at 10 ng/mL, and 7% at 100 ng/mL. Similar values for inter- and intra-assay precision were obtained for nonivamide and dihydrocapsaicin. This method was used to assay for capsaicinoids in blood and tissue samples collected from rats exposed to capsaicinoids via nose-only inhalation. The concentration of capsaicin in these samples ranged from < 1.0 to 90.4 ng/mL in the blood, < 5.0 to 167 pg/mg in the lung, and < 2.0 to 3.4 pg/mg in the liver.