高效液相色谱法测定人血浆中的芦氟沙星

 建立了测定人血浆中芦氟沙星质量浓度的高效液相色谱法 ,血浆用二氯甲烷提取 3次 ,以 UltrasphereODS(4.6mm i.d.× 2 5 0 mm)为色谱柱 ,流动相为甲醇 -1 0 mmol/L 溴化四丁铵 -三乙胺 (体积比为 3 2∶ 68∶0 .5 ) ,用磷酸调 p H2 .8,检测波长 2 95 nm,流速为 1 .2 m L/min,以培氟沙星为内标。血浆中芦氟沙星的线性范围为 0 .1～ 1 0 mg/L ,最低检测质量浓度为 0 .0 5 mg/L ,回收率为 99.7% ,日内、日间 RSD分别为 2 .3 3 %和3 .83 %。方法简便、快速、准确 ,适用于人血浆中芦氟沙星质量浓度的测定。     

固相萃取和高效液相色谱相结合快速测定苦瓜甙A的含量(英文)

 建立了一个快速、简单、准确的固相萃取和高效液相色谱相结合的测定苦瓜甙A含量的方法。样品经石墨碳固相萃取管 (3mL/ 2 5 0mg)纯化后以高效液相色谱检测。色谱柱为C18,流动相为V(乙腈 )∶V(甲醇 )∶V(5 0mmol/L磷酸二氢钾缓冲液 ) =2 5∶2 0∶6 0 ,流速为 0 .8mL/min ,检测波长为 2 0 8nm。标准曲线自 10mg/L到 10 0 0mg/L呈线形关系 (r2 =0 .9992 )。该方法具有很好的重现性 ,日内或日间的相对标准偏差和相对平均误差均小于 10 %。样品回收率大于 90 %。     

高效液相色谱法测定α-萘乙酸

 采用高效液相色谱法 ,以HypersilC1 8( 4 6mmi d × 2 50mm ,5μm)为色谱柱 ,甲醇 水 磷酸 (体积比为 60∶40∶0 35,pH 3～ 4)为流动相 ,检测波长为 2 72nm ,测定了α 萘乙酸的质量分数。在 1 6mg/L～1 0 0 0mg/L时 ,质量浓度与峰面积线性关系良好 (r =0 9997) ,精密度RSD为 0 8% (n =5)。方法简便 ,准确。     

高效液相法测定注射用赖氨匹林中的阿司匹林及游离水杨酸

 建立了高效液相法 (HPLC)同时测定注射用赖氨匹林中阿司匹林和游离水杨酸含量的方法。采用的柱为HypersilBDSC18柱 ,流动相为甲醇 水 冰醋酸 (体积比为 35∶6 5∶3) ,检测波长为 2 80nm。阿司匹林和水杨酸的质量浓度分别为 0 0 2 8g/L～ 0 14 1g/L和 0 77mg/L～ 3 85mg/L时线性关系良好 ,其线性相关系数分别为0 9999和 0 9998;加样回收率分别为 99 2 7% (RSD =0 8% )及 99 6 1% (RSD =1 3% )。     

流动注射化学发光法测定盐酸羟苄唑

基于在碱性条件下盐酸羟苄唑能够与鲁米诺产生化学发光的现象,建立了流动注射化学发光测定盐酸羟苄唑的新方法。盐酸羟苄唑的浓度在8×10-7~1×10-4mol/L范围内与化学发光强度呈良好的线性关系,方法的(3σ)检出限为3×10-7mol/L,对1×10-5mol/L的盐酸羟苄唑连续11次测定的相对标准偏差为1.7%,回收率为96%~103%。已用于滴眼液中盐酸羟苄唑的测定。     

反相高效液相色谱法测定3种中成药中的葛根素

 建立了测定小儿清感灵片、步长新脑心通胶囊和感冒清热颗粒 3种中成药中葛根素含量的反相高效液相色谱方法。采用APEXODS色谱柱 ,以醋酸铵缓冲液 (10 0mmol/L ,pH 5 0 ) 甲醇 (体积比为 75∶2 5 )的混合溶液为流动相 ,检测波长为 2 5 0nm ,流速为 0 8mL/min。葛根素在 2mg/L～ 2 0mg/L时其色谱峰面积与质量浓度的线性关系良好 (r =0 9999) ;上述 3种中成药中的葛根素含量分别为 3 48mg/g ,1 0 8mg/ g及 1 5 2mg/ g(蔗糖型 ) ;其加样回收率分别为 99 0 % ,93 4%和 97 5 %。该法简便、快速、专属性强 ,可以作为多种中药制剂中葛根素含量的测定方法。     

1-[2,3,5-三氮唑偶氮]-2-萘酚的合成及其与镉显色反应研究

合成了 1 -[2 ,3 ,5-三氮唑偶氮 ]-2 -萘酚 (简称 TNAN) ,研究了它与镉显色反应。结果表明 :在 Triton X-1 0 0存在下 ,p H7.0～ 8.7时 Cd( )与试剂形成 1∶ 2的红色络合物 ,ε=1 .79× 1 0 5L· mol- 1· cm- 1,镉浓度在 0～ 0 .8mg/ L范围内服从比耳定律。可用于水样和发样中徽量镉的测定     

柱切换-荧光检测反相高效液相色谱法测定血浆中特布他林浓度

采用柱切换技术 荧光检测反相高效液相色谱法测定血浆中特布他林 (TB)浓度。使用LunaC8( 2 )和KromasilC18为分析柱 ( 1 5 0mm× 4.6mm ,5 μm)和预处理柱 ( 2 5mm× 4.6mm ,5 μm) ,流动相分别为pH 3 0 ,0 .0 3 3mol/L磷酸盐缓冲液∶甲醇∶乙腈 ( 92∶7∶1 )和水∶甲醇∶乙腈 ( 97∶2∶1 ) ,流速均为 1 .0ml/L。血浆样品经乙腈沉淀蛋白后进样 ,切换时间为 3 .2～ 4.2min。荧光检测 ,λex为 2 80nm ,λem为 3 0 9nm。以沙丁胺醇作内标 ,按内标法定量。标准曲线线性范围为 0 .8～ 3 2 μg/L ;最低定量限为 0 .8μg/L;TB和内标的保留时间分别为 8.7和 9.3min;日内RSD小于 4% ,日间RSD小于 9% ,方法回收率在 93 %～ 1 1 2 %。     

反相高效液相色谱法测定小鼠血浆及组织中的阿昔洛韦浓度

 建立了测定小鼠血浆、肝、肾、脾、肺等组织中阿昔洛韦 (ACV)浓度的高效液相色谱法。色谱柱为HypersilODS ,流动相为甲醇 水 冰醋酸 (体积比为 1∶99∶0 5 )混合溶液 ,流速为 1 5mL/min ,检测波长为 2 5 2nm。ACV血浆最低检测浓度为 2 0 μg/L ,各组织最低检测浓度为 5 0ng/g。血浆及组织匀浆中的ACV浓度在 0 1mg/L～ 4mg/L及 0 1μg/g～ 4μg/ g时线性关系良好 (r >0 99)。血浆及肝匀浆中的ACV回收率分别为 97 5 %～ 10 0 0 %和 10 0 0 %～ 10 6 0 % (n =5 )。该法精密度高 ,方便 ,快捷 。     

亚种间杂交稻内源激素的高效液相测定法

 建立了一种快速、提取率高的从植物中提取内源激素的样品处理方法 ,并研究了高效液相法测定亚种间杂交稻的 4种内源激素 :赤霉素 (GA3 )、3 吲哚乙酸 (IAA)、玉米素 (Z)和脱落酸 (ABA)的条件。采用WatersC18反相柱 (4 6mmi.d .× 2 5 0mm ,5 μm) ,SPD 6AV紫外检测器。以甲醇 水 乙酸 (体积比为 45∶5 4 2∶0 8)溶液为流动相 ,流速 1 0mL/min ;进样量 2 0 μL ;检测波长 2 5 4nm ;选用外标法进行定量测定。其回收率高 ,检出限分别为GA3 0 5mg/L ,IAA 0 1mg/L ,Z 0 3mg/L ,ABA 0 0 3mg/L。该法快速、灵敏、准确。     

Determination of bifonazole and identification of its photocatalytic degradation products using UPLC‐MS/MS

The main goal of the presented work was to investigate the effect of ZnO or/and TiO₂ on the stability of bifonazole in solutions under UVA irradiation. To this end, a simple and reproducible UPLC method for the determination of bifonazole in the presence of its photocatalytic degradation products was developed. Linearity was studied in the range of 0.0046–0.15 mg mL⁻¹ with a determination coefficient of 0.9996. Bifonazole underwent a photocatalytic degradation process under the experimental conditions used. Comparative studies showed that combination of TiO₂/ZnO (1:1 w /w) was a more effective catalyst than TiO₂ or ZnO with a degradation rate of up to 67.57% after 24 h of irradiation. Further, kinetic analyses indicated that the photocatalytic degradation of bifonazole in the mixture of TiO₂/ZnO can be described by a pseudo‐first order reaction. Statistical comparison clearly indicated that the presence of TiO₂/ZnO also affected the stability of bifonazole from a cream preparation after 15 h of UVA exposure (p < 0.05). Ten photodegradation products of bifonazole were identified for the first time and their plausible fragmentation pathways, derived from MS/MS data, were proposed. The main pathway in the photocatalytic transformation of bifonazole in the presence of ZnO or/and TiO₂ involves hydroxylation of the methanetriyl group and/or adjacent phenyl rings and cleavage of the imidazole moiety.     

Simultaneous determination of bifonazole and tinctures of calendula flower in pharmaceutical creams by reversed-phase liquid chromatography

The aim of this research was to develop and validate a sensitive, rapid, easy, and precise reversed-phase liquid chromatography (LC) method for stability studies of bifonazole (I) formulated with tinctures of calendula flower (II). The method was especially developed for the analysis and quantitative determination of I and II in pure and combined forms in cream pharmaceutical formulations without using gradient elution and at room temperature. The influence on the stability of compound I of temperature, artificial radiation, and drug II used for the new pharmaceutical design was evaluated. The LC separation was carried out using a Supelcosil LC-18 column (25 cm x 4.6 mm id, 5 microm particle size); the mobile phase was composed of methanol-0.1 M ammonium acetate buffer (85 + 15, v/v) pumped isocratically at a flow rate of 1 mL/min; and ultraviolet detection was at 254 nm. The analysis time was less than 10 min. Calibration graphs were found to be linear in the 0.125-0.375 mg/mL (rI = 0.9991) and 0.639-1.916 mg/mL (rII = 0.9995) ranges for I and II, respectively. The linearity, precision, recovery, and limits of detection and quantification were satisfactory for I and II. The results obtained suggested that the developed LC method is selective and specific for the analysis of I and II in pharmaceutical products, and that it can be applied to stability studies.     

High-performance thin-layer chromatography determination of some antimycotic imidazole derivatives and preservatives in medicinal creams and a gel

Simple and reliable thin-layer chromatography-densitometry methods for determination of antimycotics (bifonazole, clotrimazole, and miconazole) and preservatives (benzyl alcohol and benzoic acid) were developed. The pairs bifonazole/benzyl alcohol, clotrimazole/benzyl alcohol, and miconazole/benzoic acid were determined simultaneously. The following mobile phases were used: ethyl acetate-n-heptane-methanoldiethylamine (3 + 4.5 + 1 + 0.2, v/v/v/v) for bifonazole and benzyl alcohol; n-butyl acetate-n-heptane-methanol-dietylamine (3 + 4.5 + 1 + 0.2, v/v/v/v) for clotrimazole and benzyl alcohol; and n-butyl acetate-carbon tetrachloride-methanol-diethylamine (3 + 6 + 2.5 + 0.5, v/v/v/v) for miconazole and benzoic acid. The chromatographic zones on silica gel plates were scanned in the reflectance/absorbance mode at 230 nm (bifonazole, benzyl alcohol, miconazole, and benzoic acid) and 210 nm (clotrimazole and benzyl alcohol). The recovery for all substances ranged from 98.7 to 100.7%. The limits of detection and quantitation were 0.03 to 0.2 microg and 0.1 to 0.5 microg/spot, respectively. The proposed methods were applied for determination of antimycotics and preservatives in commercially available pharmaceuticals.     

Simultaneous Determination of Bifonazole and Benzyl Alcohol in Pharmaceutical Formulations by Reverse-Phase HPLC

A simple, precise and sensitive reverse-phase high performance liquid chromatographic (RP-HPLC) method has been developed for the quantitation of bifonazole, an imidazole antifungal, simultaneously with benzyl alcohol, used as preservative, in pharmaceutical formulations. Method employed Zorbax Eclipse XDB-C18 (250×4.6 mm i.d., 5 m) column, methanol - ammonium acetate (pH 2; 65 mM) (65:35, v/v, pH^* 3.6) as mobile phase with flow rate of 1 mL min^–1 and variable UV detection at 220 and 252 nm. The proposed method was validated by testing its linearity, selectivity, recovery, repeatability, LOD/LOQ values and it was successfully employed for the determination of bifonazole and benzyl alcohol in pharmaceutical cream-based formulations.     

Bifonazole-β-cyclodextrin Inclusion Complexes. Thermal analysis and X-ray powder diffraction study

The complexation of bifonazole, an antimycotic hydrophobic imidazole derivative, with β-cyclodextrin (β-CD) was investigated in solid phase, using the following complementary techniques: differential scanning calorimetry (DSC), thermogravimetric analysis (TG) and X-ray powder diffractometry. The β-CD-bifonazole samples were prepared in both aqueous medium by coprecipitation and in solid state by kneading method and the β-CD-bifonazole binary diagrams were drawn. The experimental results demonstrate the formation of two binary compounds, β-CD-bifonazole and (β-CD)_x bifonazole (x =2 or 4). The first compound may be an inclusion compound and the second a crystallized compound, in which the bifonazole is not necessarily included in the cyclodextrin internal cavity. This revised version was published online in July 2006 with corrections to the Cover Date.     

高效液相色谱法测定萨拉沙星

采用高效液相色谱法测定了萨拉沙星。色谱柱为μ－BondapakTMC18柱（3．9mm×300mm）,流动相为V（乙腈）：V（甲醇）：V（2mmol／L磷酸,用三乙胺调pH3．5）＝30：5：65,用二极管阵列检测器检测,检测波长278nm,得到了满意的分离效果。     

全二维气相色谱-质谱法检测天然奶油和人造奶油中的脂肪酸

建立了天然奶油和人造奶油中37种脂肪酸的全二维气相色谱-质谱检测方法。样品经甲苯提取、乙酰氯-甲醇（1∶9,v/v）溶液甲酯化衍生后,以DB-5柱（30 m×0.25 mm×0.25 μm）为一维柱、BPX-50柱（2.5 m×0.1 mm×0.25 μm）为二维柱进行分离。升温程序为50℃保持2 min,以20℃/min升温至180℃,以2.5℃/min升温至250℃,以3℃/min升温至300℃,保持5 min。在调制周期为5 s、扫描范围为m/z 40~385的条件下,奶油中37种脂肪酸得到了有效分离和准确测定。将该方法应用于实际样品的分析,检测结果比传统的气相色谱法更灵敏,脂肪酸组成也更丰富,可有效鉴别不同种类奶油的差异成分。该方法不仅为奶油中脂肪酸成分分析提供了新的技术手段,同时在保障奶油的质量安全、鉴别掺假伪劣等过程中发挥重要作用。     

反相高效液相色谱法测定肌醇

 研究了用反相高效液相色谱测定肌醇的新方法。所用色谱柱为Shim-PackCLC-C18柱,以V(乙腈)∶V(水)=10∶90的溶液为流动相,流速为1.0mL/min,检测波长为196nm。测定结果的相对标准偏差为0.8%。方法简便、快速、准确,适用于肌醇产品的定量测定。     

高效液相色谱法测定20％增效噻枯唑可溶性粉剂中噻枯唑含量

建立了20％增效可溶性噻枯唑（MBAMT）粉剂中有效成分MBAMT的高效液相色(HPLC)分析方法。采用硅胶柱,正已烷：无水乙醇＝9：2（V／V）为流动相,所得结果良好,平均回收率为93．75％,变异系数为2．18％。方法简易,快速、准确,已用于产品质检。     

Gas chromatographic-mass spectrometric determination of two new antimycotic agents, 1-[(5-chloro-2-benzofuranyl)(2-chlorophenyl)methyl]-1H-imidazole and 1-[(5-bromo-2-benzofuranyl)phenylmethyl]-1H-imidazole, in rabbit plasma following topical administration: a preliminary comparison with bifonazole

A method for the analysis of the antimycotic drugs 1-[(5-chloro-2-benzofuranyl)(2-chlorophenyl)methyl]-1H-imidazole, 1-[(5-bromo-2-benzofuranyl)phenylmethyl]-1H-imidazole and bifonazole in rabbit plasma, employing gas chromatography-mass spectrometry with selected-ion monitoring, was developed. The procedure involved single-step purification of the biological matrix via liquid-liquid extraction on Extrelut columns and use of a carrier substance to minimize the negative effects of adsorption sites during the gas chromatographic process. The limits of detection ranged from 0.1 to 1.4 ng/ml, starting from a 200-microliter sample. The method was applied to a preliminary evaluation of percutaneous absorption of both drugs in the rabbit after a single administration, in comparison with bifonazole.