HPLC法测定苦瓜清脂素胶囊中盐酸西布曲明

建立高效液相色谱法测定盐酸西布曲明的含量.色谱柱为Venusil MP C18,流动相为含0.1%甲酸的20 mmol/L醋酸铵-甲醇(35∶ 65).检测波长为224 nm,流速为1.0 ml/min.盐酸西布曲明在0.0225～0.225 mg/ml范围内与峰面积线性关系良好(r=0.9998);平均回收率为98.87%,RSD为0.65%(n=6).本方法简便、准确、灵敏、重现性好,可作为盐酸西布曲明的含量测定方法.     

HPLC法同时测定复方可待因口服溶液中磷酸可待因、盐酸麻黄碱、盐酸曲普利啶的含量

目的 建立同时测定复方可待因口服溶液中磷酸可待因、盐酸麻黄碱、盐酸曲普利啶3组分含量的高效液相色谱法。方法 采用Hypersil-BDS CN柱,流动相为乙腈-0.4％乙酸铵溶液-三乙胺(30:70:0.2),流速为1.0 ml/min,检测波长257nm,外标法计算。结果 线性范围分别是磷酸可待因125-1 000 μg/ml,r=0.9999,盐酸麻黄碱75-600μg/ml,r=0.9996;盐酸曲普利啶18-140 μg/ml,r=0.9997。回收率分别为磷酸可待因99.9％、盐酸麻黄碱99.7％、盐酸曲普利啶100.3％。结论 本方法分离效果好,辅料无干扰,快速,简便,适合于该制剂3组分的同时测定。     

HPLC法检测减肥类保健食品中非法添加的酚酞和盐酸西布曲明

目的:建立高效液相色谱法检测减肥类保健食品中非法添加的酚酞和盐酸西布曲明。方法:采用高效液相色谱法,色谱柱为Agilent TC-C18色谱柱(150 mm×4.6 mm,5μm),流动相为0.02 mol/L乙酸铵溶液(用乙酸调节p H至4.0)-甲醇(45∶55),流速为1.0 ml/min,柱温为35℃,检测波长为225 nm。结果:酚酞和盐酸西布曲明分别在10.77~107.70μg/ml(r=0.999 9)和11.15~111.50μg/ml(r=0.999 9)范围内,浓度与其峰面积呈良好线性关系,平均回收率分别为99.37%(RSD为0.73%)和98.97%(RSD为0.60%)。结论:本方法简便易行、准确可靠,可用于检测减肥类保健食品中非法添加的酚酞和盐酸西布曲明。     

RP-HPLC法测定盐酸西布曲明片的含量

采用反相高效液相色谱法测定盐酸西布曲明片中盐酸西布曲明的含量 ;流动相为甲醇 - 0 .0 5 mol/L磷酸二氢钾 (5 5∶ 4 5 ,用磷酸调节 p H至 3.0± 0 .1) ;检测波长为 2 2 3nm;在 10 μg/ml～ 2 5 0 μg/ml范围内 ,线性关系良好 (r =0 .9999) ;平均回收率为 10 0 .1% (n =9) ,RSD为 0 .6%。     

HPLC法同时测定复方可待因口服溶液中磷酸可待因、盐酸麻黄碱、盐酸曲普利啶的含量

目的建立同时测定复方可待因口服溶液中磷酸可待因、盐酸麻黄碱、盐酸曲普利啶3组分含量的高效液相色谱法.方法采用Hypersil-BDS CN柱,流动相为乙腈-0.4%乙酸铵溶液-三乙胺(30:70:0.2),流速为1.0 ml/min,检测波长257nm,外标法计算.结果线性范围分别是磷酸可待因125～1 000μg/ml,r=0.9999,盐酸麻黄碱75～600μg/ml,r=0.9996;盐酸曲普利啶18～140 μg/ml,r=0.9997.回收率分别为磷酸可待因99.9%、盐酸麻黄碱99.7%、盐酸曲普利啶100.3%.结论本方法分离效果好,辅料无干扰,快速,简便,适合于该制剂3组分的同时测定.     

高效液相色谱法测定氨酚曲麻片中盐酸曲普利啶的含量

目的改进氨酚曲麻片中盐酸曲普利啶含量的测定方法。方法采用高效液相色谱法,色谱柱为HypersilBDSC18,流动相为甲醇-0.4%醋酸铵溶液-三乙胺(70∶30∶0.1),流速为1ml/min,检测波长为233nm,进样量为10μl。结果盐酸曲普利啶检测浓度在28.8~86.3μg/ml范围内与峰面积积分值线性关系良好(r=0.9998),平均回收率为100.5%(RSD=0.5%)。结论本方法简便、准确度高、重现性好,可用于本品的含量测定与质量控制。     

RP-HPLC法测定盐酸曲美他嗪缓释片的含量

目的:建立测定盐酸曲美他嗪缓释片含量的方法。方法:采用反相高效液相色谱法。色谱柱为Diamonsil?C18,流动相为庚烷磺酸钠溶液(取无水庚烷磺酸钠5.05 g,加磷酸3 ml,加水稀释至2 000 ml)-甲醇-乙腈(55∶36∶9,V/V/V),流速为1.0 ml/min,柱温为30℃,检测波长为210 nm,进样量为20μl。结果:盐酸曲美他嗪检测质量浓度在0.02².0 mg/ml范围内与峰面积积分值呈良好的线性良好(r=0.999 9);精密度、稳定性、重复性试验的RSD≤0.2%;平均加样回收率为100.08%,RSD=0.2%(n=9)。结论:该方法操作简单、重复性好、专属性强,可用于控制盐酸曲美他嗪缓释片的质量。     

高效液相色谱法测定盐酸西布曲明滴丸的含量

目的用高效液相色谱法测定盐酸西布曲明滴丸含量,为该滴丸的含量测定提供检测方法,制订质量控制标准。方法用十八烷基硅烷键合硅胶为填充剂,以磷酸二氢钾溶液(取磷酸二氢钾2.72 g,加水900 mL溶解,加三乙胺10 mL,用磷酸调节pH至3.0,加水稀释至1 000 mL)-甲醇(3∶7)为流动相,流速为1.0 mL/min,检测波长为223 nm。结果盐酸西布曲明质量浓度在10.0～499.0μg/mL范围内与峰面积线性关系良好,r=0.999 98。结论该法简便、准确、专属性好,可用于盐酸西布曲明滴丸的含量测定。     

RP-HPLC法同时测定复方曲安奈德乳膏中醋酸曲安奈德和盐酸苯海拉明的含量

目的:建立同时测定复方曲安奈德乳膏中醋酸曲安奈德和盐酸苯海拉明含量的方法。方法:采用反相高效液相色谱法。色谱柱为SunFireC18,流动相为甲醇-水(含三乙胺,磷酸调pH为7.2)(70:30,V/V),流速为1.0ml/min,检测波长为230nm,柱温为30℃。结果:醋酸曲安奈德和盐酸苯海拉明检测质量浓度线性范围分别为0.008～0.048mg/m(lr=0.9990)、0.0484～0.2904mg/m(lr=0.9999);平均回收率分别为99.0%(RSD=1.1%,n=9)、98.8%(RSD=1.6%,n=9)。结论:该方法简便、快速、准确,可用于复方曲安奈德乳膏的质量控制。     

减肥类保健食品中非法添加盐酸西布曲明的快速检测

目的建立检测减肥类保健食品中非法添加盐酸西布曲明的快速定性检测方法。方法采用薄层色谱法、高效液相色谱-二极管阵列检测器法进行定性鉴别,并采用高效液相色谱法测定其中盐酸西布曲明的含量。结果在试验的10种市售样品(含赠品)中,其中8个品种(含赠品)中被检测到掺有盐酸西布曲明。结论该方法选择性强、灵敏度高,可作为分析检测减肥类保健食品中非法添加盐酸西布曲明的比较有效的方法。     

Simultaneous determination of zonisamide, carbamazepine and carbamazepine-10,11-epoxide in infant serum by high-performance liquid chromatography

This study developed a simple method for the simultaneous determination of zonisamide (ZNS), carbamazepine (CBZ) and its active metabolite, carbamazepine-10,11-epoxide (CBZE) in infant serum using reversed-phase high-performance liquid chromatograph (HPLC). The method involves a single-step protein precipitation procedure that uses no solid-phase or liquid-liquid extraction. The HPLC separation was carried out on a Cadenza CD-C18 column (3 microm, 4.6 mm x 150 mm) with potassium phosphate buffer (pH 4.6; 25 mM)-methanol-acetonitrile (65:20:15 (v/v/v)) as a mobile phase at a 1.0 ml/min flow rate: ZNS was detectable using a UV detector at 235 nm, and both CBZ and CBZE were at 215 nm. The quantification limits were established in accordance with each therapeutic range at 2.5 microg/ml for ZNS, 0.5 microg/ml for CBZ, and 0.25 microg/ml for CBZE. The respective coefficients of variation were 1.3-6.0% and 2.2-7.7% for the intra- and inter-assay.     

HPLC法测定桂林西瓜霜中盐酸小檗碱的含量

目的建立HPLC法测定桂林西瓜霜中盐酸小檗碱的含量。方法色谱柱c,。柱（4．6mm×260mm,5μm）,流动相：乙腈m．05mol／LNaH2P04（H]P04调pH至3．0）-0．025mol／LSDS（50：25：25）;检测波长：346nm;流速：1．0mL／min;柱温：室温。结果盐酸小檗碱在0．0021—0．01477mg／mI浓度范围内与峰面积呈良好的线性关系,其回归方程为Y=1．705×10^6X＋65．56,r=0．9998,平均回收率为99．39％,RSD=1．90％。结论本方法操作简便,重现性好,精密度好,可以用来控制本制剂的质量。     

Simultaneous quantitative determination of metoprolol, atorvastatin and ramipril in capsules by a validated stability-indicating RP-UPLC method

A simple ultra performance liquid chromatographic (UPLC) method has been developed for the simultaneous estimation of Metoprolol (MT), Atorvastatin (AT) and Ramipril (RM) from capsule dosage form. The method was developed using Zorbax® XDB-C18 (4.6 mm × 50 mm, 1.8 μm) column with a mobile phase consisting of 0.06% ortho phosphoric acid in Milli Q® water having an ion pair reagent, 0.0045 M Sodium lauryl sulphate as buffer, at ratio of buffer: Acetonitrile (50:50 v/v), at 55°C column temperature with a flow rate of 1.0 ml/min. Detection was carried out with ultra-violet detection at 210 nm for RM, MT and AT respectively. The retention times were about 1.3, 2.1 and 2.6 min for MT, AT and RM respectively, the method was validated for linearity, accuracy, precision, specificity, robustness and ruggedness. The % mean recoveries are 101.9, 102.1 and 101.4 for MT, AT and RM respectively. The method was found to be rugged and robust and can be successfully used to determine the three drugs and its combinations.     

高效液相色谱法测定人血浆中盐酸氨溴索的浓度

目的 建立HPLC测定人血浆中盐酸氨溴索含量的方法。 方法 选用Diamonsil-C₁₈柱(200 mm×4.6 mm,5μm),流动相:甲醇-0.01 mol/L磷酸盐缓冲液(pH 7.0)-四氢呋喃(700:320:25,v/v/v),流速:1.2 ml/min,检测波长:242 nm,柱温:室温。 结果 该方法低、中、高3种浓度的提取回收率为88.2％ ~104.8％ ,日内、日间相对标准差为2.7％~5.3％(n=6),在10.2~610.8 ng/ml范     

Ion-Pairing Reverse-Phase High Performance Liquid Chromatography Method for Simultaneous Estimation of Atenolol and Indapamide in Bulk and Combined Dosage Form

A sensitive, accurate, precise and validated ion-pairing reverse-phase liquid chromatographic method for the quantitative determination of atenolol and indapamide in bulk and tablet dosage form was developed. The proposed ion-pairing reverse-phase high performance liquid chromatography method utilises C₁₈ column with 5 μm, 150×4.6 mm i.d. column and mobile phase consisting of 0.1% w/v solution of octane sulphonic acid, sodium salt and methanol (55:45 v/v), (pH 2.8) and ultraviolet detection at 235 nm. A linearity range of 1-250 μg/ml and 1-25 μg/ml for atenolol and indapamide, respectively, was obtained. The mean recoveries are 100.48 and 99.82% for atenolol and indapamide, respectively. The method was validated as per International Conference on Harmonization guidelines.     

A simple and rapid high-performance liquid chromatographic method for the determination of bisoprolol fumarate and hydrochlorothiazide in a tablet dosage form

A simple and precise high performance liquid chromatographic method has been developed and validated for the simultaneous determination of bisoprolol fumarate (BF), and hydrochlorothiazide (HCTZ) in a tablet formulation. Chromatography was carried out at 25 degrees C on a 4.6 mm x 250 mm, 5 microm cyano column with the isocratic mobile phase of 0.1M aqueous phosphate buffer, acetonitrile and tetrahydrofuran (85:10:5, v/v/v) at a flow rate of 1.0 ml/min. The UV detection was carried out at 225 nm. HCTZ and BF were separated in less than 10 min with good resolution and minimal tailing, without interference of excipients. The method was validated according to ICH guidelines and the acceptance criteria for accuracy, precision, linearity, specificity and system suitability were met in all cases. The method was linear in the range of 50-150 microg/ml for BF and 125-375 microg/ml for HCTZ.     

Simultaneous Estimation of Nebivolol Hydrochloride and Valsartan using RP HPLC

In this study, a rapid, precise, accurate, specific and sensitive ion-paired reverse phase liquid chromatographic method has been developed for the simultaneous estimation of nebivolol hydrochloride and valsartan in their capsule formulation. The chromatographic method was standardized using a HIQ sil C₁₈ column (250×4.6 mm i.d., 5 μm particle size) with UV detection at 289 nm and flow rate of 1 ml/min. The mobile phase consisting of methanol:water (80:20 v/v) with addition of 0.1 percent 1-hexanesulfonic acid monohydrate sodium salt as an ion-pairing reagent was selected. The method was validated and produced accurate and precise results for estimation of the two drugs.     

Determination of fluocortolone pivalate and fluocortolone hexanoate in suppositories using reverse-phase HPLC

Fluocortolone and its esters are synthetic corticosteroids used topically in the treatment of various skin disorders. A method that can be successfully used for the separation and determination of fluocortolone pivalate and fluocortolone hexanoate in suppositories was developed. This method is based on reverse-phase HPLC on Supelcosil LC-18 (25 cm x 4.6 mm, 5 microns), using methanol-acetonitrile-water-glacial acetic acid (17:46:37:0.4 v/v/v/v) as mobile phase at a flow rate of 3.0 ml/min. Detection was carried out using a UV detector at 238 nm. The method developed was validated, and calibration curves were established dependent on peak area. The validated ranges for fluocortolone pivalate and fluocortolone hexanoate are 15-305 micrograms/ml (r = 0.9995) and 15-315 micrograms/ml (r = 0.9996), respectively. The limits of detection and the limits of quantification for both esters were also determined.     

Simultaneous determination of cinnarizine and domepiridone maleate from tablet dosage form by reverse phase ion pair high performance liquid chromatography

A new simple, precise, rapid and selective reverse phase ion pair high performance liquid chromatography (HPLC-RP) method has been developed for the simultaneous determination of cinnarizine (CINN) and domepiridone maleate (DOME) from tablets using acetonitrile–methanol–water–0.1 N sulfuric acid (37:10:48:5 v/v/v/v) containing sodium lauryl sulfate (0.01 M), as a mobile phase and a Machery Nagel nitrile column (10 μ, 25 cm×4.0 mm i.d.) as the stationary phase. The flow of mobile phase through the column was kept at 1.0 ml min⁻¹ through out the analysis. Detection was carried out using a UV detector at 225 nm. The retention times for CINN and DOME were 4.73 and 9.41 min, respectively. The linearity range and percentage recoveries for CINN and DOME were 4–1000 and 60–750 μg ml⁻¹ and 99.90 and 99.60%, respectively.