转换曲线分光光度法测定复方磺胺甲(口恶)唑片的含量

目的:研究复方磺胺甲(口恶)唑片更简便的含量测定方法.方法:用转换曲线分光光度法原理,以乙醇-0.1mol·L-1盐酸(1∶1)为溶剂,直接测定复方磺胺甲(口恶)唑片中SMZ和TMP的含量.结果:SMZ及TMP的平均回收率和RSD(n=6)分别为(100.0±0.22)%和(99.88±0.90)%.结论:方法简便、快速、准确.     

HPLC法测定复方磺胺甲噁唑颗粒剂的含量

目的:采用HPLC法同时测定复方磺胺甲噁唑颗粒剂中磺胺甲噁唑(SMZ)和甲氧苄啶(TMP)的含量。方法:色谱柱为ODS C_(18)柱,4.6x150mm,流动相为甲醇-磷酸盐缓冲液(pH5.90)(20:80),检测波长为240nm。结果:线性范围分别为:SMZ 20～181μg·ml~(-1),(r=0.9999);TMP 4～38μg·ml~(-1),(r=0.9999)。平均回收率分别为:SMZ100.5％(RSD=0.29％);TMP 100.3％(RSD=0.51％)。结论:本法分离度好,快速,简便,可同时测定该品中的两种组分。     

双波长系数标准加入法测定抗菌优中磺胺甲恶唑的含量

抗菌优是由磺胺类抗菌消炎药磺胺甲口恶唑 ( SMZ)和磺胺增效剂甲氧苄氨嘧啶 ( TMP)两组分组成的复方制剂。用紫外分光光度法不经分离对抗菌优中两组分或主要组分SMZ含量测定的方法在国内外已有不少报道 ,如双波长比值光谱法 [1 ] 、倍率减差双波长分光光度法 [2 ] 、吸收度线性组合法 [3] 。本文作者在参考以上文献的基础上提出双波长系数标准加入法 ,对多组分药物进行定量分析 ,并用于抗菌优中 SMZ的含量测定 ,获得了满意的结果。1　仪器和试剂日本岛津分光光度计 ( U V- 2 60 ) ,磺胺甲口恶唑和甲氧苄氨嘧啶均符合药典规定标准 (山…     

双波长一元线性回归分光光度法同时测定复方磺胺甲噁唑片中两组分含量

本文采用双波长一元线性回归分光光度法同时测定了复方磺胺甲噁唑片中SMZ和TMP的含量,分析结果表明:平均回收率SMZ为99.9%,TMP为100.2%,变异系数SMZ为0.25%,TMP为0.76%。     

高效液相色谱法测定复方必消痰胶囊成分含量

目的建立高效液相色谱(HPLC)法测定复方必消痰胶囊中磺胺甲基异口恶唑(SMZ)、甲氧卞啶(TMP)、盐酸溴己新的含量。方法采用KF-C18(4.6mm×250mm,10μm)色谱柱;流动相:甲醇-水-0.01mol/L三乙胺甲醇溶液(95∶5∶1.5);流速:1.0m l/m in;检测波长:249nm。结果SMZ在4.56~22.8μg/m l、TMP在9.08~45.4μg/m l、盐酸溴己新在10.16~50.80μg/m l范围内呈良好线性关系(n均为5,r均为0.9999)。SMZ、TMP、盐酸溴己新的平均回收率分别为100.92%(n=9,RSD=2.03%)、99.06%(n=9,RSD=1.32%)、101.02%(n=9,RSD=0.62%)。结论本法简便、快速、准确,适用于制剂的质量分析。     

HPLC同时测定复方磺胺甲噁唑片的两个主药含量

目的建立复方磺胺甲噁唑片中磺胺甲噁唑(sohamethoxazole,SMZ)和甲氧苄啶(trimethoprim,TMP)的HPLC测定方法。方法采用高效掖相色谱法,色谱柱:waters C18(4μm,3.9mm×150mm)柱,流动相为乙腈-磷酸缓冲液(pH6.8±0.1),(12∶88),检测波长为240nm。结果在优化的色谱条件下,SMZ和TMP完全分离,片剂辅料不干扰测定,SMZ在20～100μg/mL范围内呈良好线性关系(r=0.9999),TMP在4～20μg/mL范围内呈良好线性关系(r=0.9999)。ASD<1.5%。结论该法结果准确、简便、快速、专属性强,重复性好,敏感度高,适用于复方磺胺甲噁唑片的含量测定。     

副伤寒沙门氏菌耐药性与菌株质粒的监测

目的掌握副伤寒沙门氏菌的耐药情况,探讨其耐药机制,合理使用抗生素。方法对1997～2001年从桂林地区分离到的292株副伤寒沙门氏菌进行药敏实验和质粒检测。结果292株副伤寒沙门氏菌对呋喃唑酮、头孢氨苄、头孢唑林、头孢拉定敏感率达100%,对复方磺胺甲口恶唑的耐药率为80.0%,磺胺甲异口恶唑为85.6%,对此两种抗生素的耐药性有逐年增高的趋势。菌株多重耐药最多可达4～6种,耐药类型以磺胺甲异口恶唑、复方磺胺甲口恶唑、青霉素、红霉素为主。85.6%(250/292)的菌株可检出带有89.3Mu的大分子质粒,质粒检出率与耐药种类呈正相关(t=4.78,P<0.05),所有耐磺胺甲异口恶唑和复方磺胺甲口恶唑的菌株均能检出该质粒,而29株敏感株则未能检出质粒。结论桂林地区副伤寒杆菌普遍对磺胺甲异口恶唑和复方磺胺甲口恶唑耐药,呋喃唑酮、头孢氨苄、头孢唑林、头孢拉定等抗生素为桂林地区治疗副伤寒的首选药物。菌株携带89.3Mu大分子质粒,与副伤寒菌株的耐药性有关。     

复方新诺明治疗细菌性痢疾(摘要)

复方新诺明(每片含 SMZ—磺胺甲基异(口恶)唑0.4克和 TMP—磺胺甲氧苄胺嘧啶0.08克)是一种新的广谱抗菌合剂。因为 SMZ 与 TMP 的体内吸收及排泄过程相似,都能在肠胃道很好的吸收,且不受食物的影响,所以它们的联合应用可以使对痢疾杆菌的抑菌作用变为杀菌作用,较其他磺胺与TMP 联用的效果为佳,并具有快速、安全有效、用法简便,近期(3—6月)无复发等优点。我们用复方新诺明治疗细菌性痢疾100例,其     

双波长系数标准加入法测定抗菌优中磺胺甲口恶唑的含量

抗菌优是由磺胺类抗菌消炎药磺胺甲口恶唑(SMZ)和磺胺增效剂甲氧苄氨嘧啶(TMP)两组分组成的复方制剂.用紫外分光光度法不经分离对抗菌优中两组分或主要组分SMZ含量测定的方法在国内外已有不少报道,如双波长比值光谱法[1]、倍率减差双波长分光光度法[2]、吸收度线性组合法[3].本文作者在参考以上文献的基础上提出双波长系数标准加入法,对多组分药物进行定量分析,并用于抗菌优中SMZ的含量测定,获得了满意的结果.     

毛细管区带电泳法测定复方磺胺甲噁唑片中两组分的含量

建立毛细管区带电泳法测定复方磺胺甲口恶唑片中磺胺甲口恶唑和甲氧苄啶含量的方法。用 2 5mmol/L硼砂缓冲液分离 ,以氯霉素为内标 ,2 14nm为测定波长。结果 :样品中二组分完全分离且呈良好线性关系 ,加样回收率分别为 10 1.0 % ( RSD =1.4 3% ) ,10 0 .3% ( RSD =1.2 8% )。     

双波长倍增差示法测定复方新诺明片含量

分别测定标准溶液和样品溶液在265及275 nm处的吸收度,根据标准溶液的吸收系数可同时计算出样品中 SMZ 和 TMP 的含量。SMZ 平均回收率与变异系数分别为100.8%,0.95%;TMP 为99.16%,0.82%。方法简便、快速。结果令人满意。     

Chemometric and derivative methods as flexible spectrophotometric approaches for dissolution and assaying tests in multicomponent tablets

Two derivative spectrophotometric (ratio derivative spectra and algorithm bivariate calibration) and a chemometric methods (partial least squares, PLS) are proposed for the simultaneous determination of binary mixtures in tablet analysis and dissolutions tests, without prior separation. These approaches are successfully applied to quantify trimethoprim (TMP) combined with sulfamethoxazole (SMX) or sulfamethazine (SMZ) or sulfafurazole (SFZ) using the information in the absorption spectra of appropriate solutions. Beer's law was obeyed in the concentration range of 0.98-17.5 microg/ml for TMP, 0.95-17.2 microg/ml for SMX, 1.16-17.5 microg/ml for SMZ and 0.97-17.4 microg/ml for SFZ. The first derivative (1D) bivariate algorithm method involves the use of four calibration curves: two for each compound at two different wavelengths, selected by Kaiser's method. Similarly, the first derivative ratio spectrophotometry employs the linear relationship between the ratio spectra of the analytes and the concentration range. The results were compared with those obtained by PLS multivariate calibration. The calibration models from PLS were pre-treated by orthogonal signal correction and evaluated by cross-validation using the 'SIMCA-P 9' software. Synthetic mixtures of TMP and sulfonamides were used in five different sets for the validity of the calibrations. Mean recoveries for derivative ratio, derivative bivariate and PLS methods were found to be between 99.7% and 102.0% for TMP, 99.4% and 100.2% for SMX, 99.3% and 101.0% for SMZ and 98.1% and 102.3% for SFZ. The calibrations of the three methods were successfully applied to the assaying and dissolution of placebo and commercial tablets without any prior separation. More than 85% of TMP, SMX and SMZ were dissolved within 15 min. For SFZ, only 85% of the compound was dissolved after 60 min. In this study, the three spectrophotometric methods can be satisfactorily used for the quantitative analysis and for dissolution tests of multicomponent dosage forms.     

HPLC法测定复方磺胺甲噁唑分散片两种成分的含量

目的建立测定复方磺胺甲噁唑分散片两种成分的高效液相色谱方法。方法采用HPLC法,kromasil C18柱（4.6×150mm,5μm）;以水-乙腈-三乙胺（800∶200∶1）（用醋酸调pH至5.9）为流动相;检测波长：240nm;流速：1.0mL.min-1;柱温：30℃。结果磺胺甲噁唑进样量在60～600μg.mL-1范围内呈良好的线性,r=0.9999;平均回收率为97.97%,RSD=0.88%;甲氧苄啶进样量在16～160μg.mL-1范围内呈良好的线性,r=0.9999;平均回收率为97.48%,RSD=0.75%。结论本方法操作简便,结果准确可靠,可用于复方磺胺甲噁唑分散片的质量控制。     

多次标准加入分光光度法同时测定复方药物中各组分含量的研究

A computational analytical method of simultaneous determination of components in compound drug without preliminary separation has been proposed. It is a matrix computation by means of multi-standard addition spectrophotometry on multi-wavelengths. The compound tablets of sulfamethoxazole was used to perform the experiment. In the experiment, the rule of error propagation for matrix computation was taken for the selection of solvent, groups of wavelengths and faction of standard addition, and the suitable concentration of standard addition was decided by test. In the case of determination for the simulated solution compound sulfamethoxazole, the recoveries for SMZ and TMP were 99.26～101.8 and 97.77～102.0%, respectively, with standard deviation of less than 0.51% and 213%, respectively. The method had been applied to the determination for compound tablets of sulfamethoxazole with satisfactory results.     

A flow injection sensor for simultaneous determination of sulfamethoxazole and trimethoprim by using Sephadex SP C-25 for continuous on-line separation and solid phase UV transduction

A flow-through sensor based on integration of spectrophotometric detection and the different kinetics of retention/elution of analytes on a solid support is proposed for the simultaneous determination of sulfamethoxazole (SMZ) and trimethoprim (TMP). The solid support (Sephadex SP C-25) fills both, a microcolumn placed on-line and the sensing microzone. The intrinsic absorbance of both compounds is monitored directly on the solid phase at 269 nm and so, no derivatization step is required. Using two alternate solutions, 10(-4) M hydrochloric acid and 0.20 M NaAc/HAc (pH 5.0) buffer, the sensor responds linearly in the measuring range of 50-250 and 10-70 microg ml(-1) with detection limits of 9.5 and 0.6 microg ml(-1) (500 microl of sample volume) for SMZ and TMP, respectively. The main advantages of the sensor are simplicity, rapidity and low reagents consumption. Its application to SMZ and TMP determination in synthetic samples and pharmaceutical preparations is demonstrated. The results obtained by the proposed method were compared with those obtained by a standard HPLC method.     

增效联磺片的体外溶出度和体内生物利用度

建立了测定体外溶出介质中磺胺嘧啶(SD)、磺胺甲噁唑(SMZ)和甲氧苄啶(TMP)及血浆中SD,SMZ,TMP和两个代谢产物N⁴-acetyl-SD和N⁴-acetyl-SMZ的反相高效液相色谱法,并对市售两种增效联磺片(片剂A和B)进行了体外溶出度和人体内生物利用度的研究。体外溶出度实验表明:两种片剂相同主药的T⁵⁰差异非常显著(P<0.001),片剂A主药的溶出比B快。生物利用度试验表明:片剂B相对于A的口服吸收分数为0.73(SD),0.78(SMZ)和0.83(TMP),口服片剂后各主药的体内过程符合表观一级吸收和一级消除的单室模型。     

Simultaneous determination of sulphamethoxazole and trimethoprim in powder mixtures by attenuated total reflection-Fourier transform infrared and multivariate calibration

A partial least-squares calibration (PLS) procedure in combination with infrared spectroscopy has been developed for simultaneous determination of sulphamethoxazole (SMZ) and trimethoprim (TMP) in raw material powder mixtures used for manufacturing commercial pharmaceutical products. Multivariate calibration modeling procedures, interval partial least squares (iPLS) and synergy partial least squares (siPLS), were applied to select a spectral range that provided the lowest prediction error in comparison to the full-spectrum model. The experimental matrix was constructed using 49 synthetic samples and 15 commercial samples. The considered concentration ranges were 400–900 mg g⁻¹ SMZ and 80–240 mg g⁻¹ TMP. Spectral data were recorded between 650 and 4000 cm⁻¹ with a 4 cm⁻¹ resolution by Fourier transform infrared spectroscopy coupled with attenuated total reflectance (ATR-FTIR) accessory. The proposed procedure was compared with conventional procedure by high performance liquid chromatography (HPLC) using 15 commercial samples containing SMZ and TMP. The results showed that PLS regression model combined to ATR-FTIR is a relatively simple, rapid and accurate procedure that could be applied to the simultaneous determination of SMZ and TMP in routine quality control of powder mixtures. A root mean square error of prediction (RMSEP) of 13.18 mg g⁻¹ for SMZ and 6.03 mg g⁻¹ for TMP was obtained after selection of better intervals by siPLS. Using the proposed procedure it is possible to analyze each sample in less than 3 min considering two replicates (excluding the grinding step). Accuracy was checked by comparison to HPLC method and agreement better than 98.8% was achieved.     

Steady-state pharmacokinetics of sulfamethoxazole and trimethorprim in man after rectal application

The pharmacokinetics of a combination of 800 mg sulfamethoxazole (SMZ) and 160 mg trimethoprim (TMP) were studied in 5 healthy male volunteers after repetitive rectal administration at constant 8-h dosing intervals. The average serum concentrations measured in steady-state between the fourth and seventh days showed a range for total SMZ of 47.86 to 63.38 microgram/ml. Free SMZ was between 40.04 and 51.42 microgram/ml and TMP between 1.44 and 2.20 microgram/ml. The ratio of total SMZ to free SMZ did not change during the course of the investigation. The pharmacokinetic parameters were derived from a simultaneous curve fitting of the Bateman function on the basis of the multiple dose equation. The values thus found for V0 and t50% correlate essentially with those found in the literature for oral administration. In addition, the final serum minimums and maximums were calculated. Extrapolation from t leads to infinity gave a serum minimum for total SMZ of 51.7 microgram/ml and 1.8 microgram/ml for TMP. The course of the curve fitting did not show an accumulative trend so that, in fact, it can be assumed that a steady-state was present.     

近红外光谱法快速分析小儿复方磺胺甲嗯唑颗粒的水分含量

目的利用近红外漫反射光谱（NIRDRS）分析技术和化学计量学方法对小儿复方磺胺甲嗯唑颗粒的水分含量进行快速定量分析。方法以全国不同企业生产的小儿复方磺胺甲嗯唑颗粒为分析对象,为扩大检测的浓度范围,通过恒温恒湿引湿的方法制得实验室制备样品,用光纤探头直接接触样品采集近红外漫反射光谱,采用偏最小二乘法（PLS）建立模型。结果小儿复方磺胺甲嗯唑颗粒水分定量分析模型由64个样本经内部交叉验证建立,42个样本用于外部验证,浓度范围为0．12％～6．15％,内部交叉验证相关系数（r）为0．9975,交叉验证均方差（RMSECV）为0．0835,外部验证均方差（RMSEP）为0．0865。结论建立的定量分析模型能对小儿复方磺胺甲嚷唑颗粒的水分含量进行准确、快速定量分析,方法简单可靠,可用于药品的现场快速分析。     

Trimethoprim/sulfamethoxazole does not affect the steady-state disposition of indinavir.

This study evaluates the safety and potential pharmacokinetic interaction between indinavir and trimethoprim/sulfamethoxazole (TMP/SMZ). In a randomized, three-period crossover fashion, 12 healthy adults received 1 week of indinavir sulfate 400 mg orally every 6 hours with placebo, TMP 160 mg/SMZ 800 mg orally every 12 hours with placebo, and indinavir sulfate with TMP/SMZ. Plasma indinavir, SMZ, and TMP concentrations were determined after the last dose of each treatment period. Concomitant administration resulted in a 17% decrease in geometric mean trough plasma indinavir concentrations (p = 0.032), an 18% increase in geometric mean AUC0-12 h and Cmax TMP values (p = 0.031 and 0.030, respectively), and a 5% increase in geometric mean AUC0-12 h SMZ values (p = 0.039). None of these effects was considered clinically significant. The combination of indinavir sulfate and TMP/SMZ is generally well tolerated, with no clinically significant pharmacokinetic interaction being noted.