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1.
Separation of fluoxetine enantiomers on five chiral stationary phases （chiralcel OD-H, chiralcel OJ-H, chiralpak AD-H, cyclobond 1 2000 DM and kromasil CHI-TBB） was investigated. The optimal mobile phase compositions of fluoxetine separation on each column were hexane/isopropanol/diethyl amine （98/2/0.2, v/v/v）, hexane/isopropanol/diethyl amine （99/1/0. l, v/v/v）, hexane/isopropanol/diethyl amine （98/2/0.2, v/v/v）, methanol/0.2% triethylamine acetic acid （TEAA） （25/75, v/v; pH 3.8） and hexane/isopropanol/diethyl amine （98/2/0.2, v/v/v）, respectively. Experimental results demonstrated that baseline separation （Rs〉1.5） of fluoxetine enantiomers was obtained on chiralcel OD-H, chiralpak AD-H, and cyclobond I 2000 DM while the best separation was obtained on the last one. The eluate orders of fluoxetine enantiomers on the columns were determined. The first eluate by chiralcel OJ-H and kromasil CHI-TBB is the S-enantiomer, while by chiralpak AD-H and cyclobond 12000 DM is the R-enantiomer. 相似文献
2.
采用高效液相色谱法,以β-环糊精为手性固定相拆分奥丁尼酮洛芬缓释胶囊中酮洛芬对映体,并对流动相中甲醇的含量、流动相的pH值、缓冲盐的浓度等色谱条件对拆分结果的影响进行了探讨.结果表明,在柱温为25℃,pH值为4.0,采用0.01 mol/L的磷酸二氢钾缓冲溶液,甲醇40%（V/V）作流动相时,奥丁尼酮洛芬缓释胶囊中的酮洛芬对映体能达到较好分离. 相似文献
3.
郭佳莉 《泉州师范学院学报》2014,(2):36-39
用邻苯二甲醛（OPA）、N-乙酰-L-半胱氨酸为衍生试剂对天冬氨酸对映体进行柱前衍生．采用ZORBAX Eclipse AAA4．6×150mm,5μm色谱柱,以0．05mol／LpH5．08的醋酸钠溶液与甲醇按57：43体积比作为流动相,流速0．5mL／min,柱温40℃下,考察高效液相色谱柱前衍生化法分离测定天冬氨酸对映体的效果．结果显示：在3．5min内分离出天冬氨酸对映体．在20～100nmol／mL线性范围内,线性关系良好,相关系数在0．99915以上,相对标准偏差在0．65％～1．70％之间．该法快速、简便、分离度高,能够完全分离DL-天冬氨酸对映体,并对其他氨基酸对映体的分离有良好的参考价值． 相似文献
4.
用微晶纤维素和甲基苯甲酰氯反应合成了手性填料纤维素-三(4-甲基苯甲酸酯)(CTMB),并涂敷于氨丙基硅胶上,制备成手性固定相(CSP)。用高效液相色谱法,在正相条件下用此手性固定相,对农药禾草灵外消旋体进行了拆分,考察了流动相组成,醇效应,温度及色谱柱长度对拆分及保留的影响,并对其在该手性柱上保留机理进行了讨论。 相似文献
5.
本文用磺化四苯基卟啉（ＴＰＰＳ_４）作柱前衍生试剂,研究了试剂与Ｃｕ（Ⅱ）、Ｚｎ（Ⅱ）的络合反应．四乙基溴化铵为离子对试剂,离子对高效液相色谱－光度法是快速分离并测定铜、锌的新方法．在 ＯＤＳ色谱柱上,用乙腈－水（２２： ７８, ｖ／ｖ）作流动相,以双波长（４１５ｎｍ和４２５ｎｍ）进行光度检测．络合物在８ｍｍ内出峰完毕,检测下限为Ｃｕ０．０９（×１０~(－３)μｇ／ｍｌ）,Ｚｎ ０．０８（× １０~(－３)μｇ／ｍｌ）．将所建立的方法用于树叶中铜和锌的测定,结果令人满意． 相似文献
6.
The enantioselective assay for S( )- and R(-)-propafenone (PPF) in human urine that developed in this work involves extraction of propafenone from human urine and using S( )-propafenone as internal standard, chiral derivatization with 2,3,4,6-tetra-O-β-D-glucopranosyl isothiocyanate, and quantitation by an RP-HPLC system with UV detection (λ=220nm). A baseline separation ofpropafenone enantiomers was achieved on a 5-μm reverse phase ODS column, with a mixture of methanol:water:glacial acetic acid (25:12:0.02,v/v) as mobile phase. There was good linear relationship from 24.9 ng/ml to 1875.0 ng/ml for both of enantiomers. The regression equations of the standard curves based on Cs-PPF (or CR-PPF ) versus ratio of As-PPF/As (or AR-PPF/As ) were y=0.0032x-0.081, (r=0.999) for S-PPF and y=0.0033x 0.0039, (r=0.998) for R-PPF,respectively. The method's limit of detection was 12.5 ng/ml for both enantiomers, and the method's limit ofquantitation was 28.2±0.52 ng/ml for S-PPF, 30.4±0.53 ng/ml for R-PPF (RSD＜8%, n=5). The analytical method yielded average recovery of 98.9% and 100.4% for S-PPF and R-PPF, respectively. The relative standard deviation was no more than 6.11% and 6.22% for S-PPF and R-PPF, respectively. The method enabled study of metabolism of S( )- and R(-)-propafenone in human urine. The results from 7 volunteers administered 150 mg racemic propafenone indicated that propafenone enantiomers undergo stereoselective metabolism and that in the human body, S( )-propafenone is metabolized more extensively than R(-)propafenone. 相似文献
7.
Chromatograms of tocopherol homologues were obtained by a column of analytical size （inner diameter （ID） 0.46 cm cm×10 cm） packed with silica gel. Adsorption isotherms and film mass-transfer coefficient were estimated from the chromatograms by using a general rate model, which considers axial dispersion, external mass-transfer and intraparticle diffusion. Based on the obtained isotherms and mass-transfer coefficient, the separation process of tocopherol homologues on simulated moving bed （SMB） was simulated using the same model. According to the simulated results, a mixture of α-, γ-, δ-tocopherols and other impurities was separated on an SMB equipment. The SMB equipment was composed of 8 columns of ID 2 cm× 1 0 cm, with 2 columns in each section. The solid phase was silica gel, and the mobile phase was n-hexane/2-propanol （99/1 by volume）. γ- and δ-tocopherols of purity greater than 98% were obtained with recovery greater than 98%. The effects of operating conditions （flow rates and switching time） on the performance of SMB were studied by both simulation and experiments. It was found that all the simulation results were quite close to the experimental results. We conclude that process development and optimization of operating conditions of SMB by simulation are feasible. 相似文献
8.
目的：建立乳酸左氧氟沙星氯化钠注射液中主药的含量测定方法。方法：采用反相高效液相色谱法。以Lichrospher5-C18为色谱柱;己烷磺酸钠-甲醇（3：1）为流动相;流速为1．0ml／min;检测波长为293nm,柱温为40℃,进样量为20u1。结果：乳酸左氧氟沙星浓度在5．0-50．0μg／ml内线性关系良好（r=0．9995）,平均回收率为99．85％。RSD为0．25％。结论：此法准确可靠,重现性好,能有效控制乳酸左氧氟沙星氯化钠注射液的质量。 相似文献
9.
对2-羟基-4-甲氧基苯乙图的高效液相色谱分析方法进行了研究。结果表明,在Spherisorb－ODS柱上,以甲醇-水（80：20,v／v）为流动相,在268mm波长下能很好地分离和检测题示物质。在药物浓度5～80mg／L范围内具有良好的线性关系,Y=8．345X—0．018,r=0．9998,检测限为0．3mg／L,平均回收率为99．7％,精密度RSD=1．3％。 相似文献
10.
11.
韦文惠 《柳州职业技术学院学报》2009,9(3):77-80
利用反相高效液相色谱法（RP—HPLC）,在Spherisorb C18柱上以乙腈-0．2g／L氨三乙酸（pH2．5）（体积比20：80）为流动相,柱温35℃,于267nm紫外检测牛奶中残留的氯霉素（CP）、金霉素（CTC）、土霉素（OTC）、四环素（TC）。考查了流动相的组成、流动相pH等因素对分离度的影响。实验条件下,四种抗生素在试验浓度范围内色谱峰面积与浓度呈现良好线性关系。四种抗生素的加标回收率分别为：土霉素为105％,四环素为90％,金霉素为82％,氯霉素为87％;检测限（SIN=3）分别为土霉素为0．35mg／L、四环素为0．30mg／L、金霉素为0．80mg／L、氯霉素为0．70mg／L。方法简单、快速,可用于奶制品中这些抗生素的检测。 相似文献
12.
采用PTC法合成了E-4,5-二取代苯基-2-吡咯烷酮,反式异构体与顺式异构体之比为973,产率高达74%,其结构用1HNMR和MS表征. 相似文献
13.
合成了3-氨基-1,3,4,5-四氢-2H-1-苯并氮杂卓-2-酮的消旋体,对所合成到的消旋体化合物进行了手性拆分实验研究,找到了以焦谷氨酸为手性拆分结晶试剂,5-硝基水杨醛为不对称结晶诱导催化剂,乙醇-水溶液为溶剂的实验条件.反应条件温和,所得手性化合物的光学纯度高,其中R（＋）-3-氨基-1,3,4,5-四氢-2H-1-苯并氮杂卓-2-酮的拆分收率为74%,[!]D＋446＂（c=1.0,CH3OH）;S（-）-3-氨基-1,3,4,5-四氢-2H-1-苯并氮杂卓-2-酮的拆分收率为71%,[!]D-443＂（c=1.0,CH3OH）. 相似文献
14.
在化学教学过程中,应用Gaussian计算程序,对顺反二氟乙烯的能量进行对比,发现两者相似。进一步探究发现,二氟乙烯的稳定性不仅受空间住阻、静电斥力大小影响,而且还与CH—CF^＊分子轨道间的电子离域有关。通过在教学中应用Gaussian程序,对化学问题进行相关深入计算,有利于培养学生严谨的学习精神与实事求是的探究学风。 相似文献
15.
Huang MZ Shentu JZ Chen JC Liu J Zhou HL 《Journal of Zhejiang University. Science. B》2008,9(2):114-120
This study presents a rapid, specific and sensitive liquid chromatography/tandem mass spectrometry (LC-MS/MS) assay for determination of risperidone (RIS) in human serum using paroxetine as an internal standard (IS). An Alltima-C 18separation. The analysis was performed by selected reaction monitoring (SRM) method, and the peak area of the m/z 411.3→ 191.1 transition for RIS was measured versus that of the m/z 330.1→192.1 transition for IS to generate the standard curves. The assay linearity of RIS was confirmed over the range 0.25～50.00 ng/ml and the limit of quantitation was 0.05 ng/ml. The linear range corresponds well with the serum concentrations of the analytes obtained in clinical pharmacokinetic studies. Intraday and interday relative standard deviations were 1.85%～9.09% and 1.56%～4.38%, respectively. The recovery of RIS from serum was in the range of 70.20%～84.50%. The method was successfully applied to investigate the bioequivalence between two kinds of tablets (test versus reference products) in 18 healthy male Chinese volunteers. The result suggests that two formulations are bioequivalent. 相似文献
16.
高效液相色谱法同时测定美白类化妆品中熊果苷和氢醌的含量 总被引：1，自引：0，他引：1
探讨了高效液相色谱法同时测定关白化妆品中熊果苷和氢醌含量的方法,先对样品进行预处理,处理液为氯仿-饱和氯化钠溶液（体积比2：1）,再选用ApolloC18柱,以甲醇-磷酸缓冲液-冰醋酸（体积比25475：1）混合液为流动相,紫外检测,波长为254nm。实验结果表明,该方法在0．01～0.2g/L时具有良好的线性;平均回收率范围为97％～98．5％;熊果苷的检出限为21μg／kg,氢醌的检出限24μg／kg。 相似文献
17.
实验采用VP-ODS色谱柱(150 mm×4.6 mm,5.0μm),以5%甲醇-10%乙腈-85%30 mM磷酸缓冲液(pH3.0,体积比)为流动相;流速为1.0 mL/min,检测波长为285 nm.该方法对13种喹诺酮类药物的线性范围为0.03～100μg/mL,最低检测限为0.001～0.03μg/mL;样品萃取回收率均大于64%,方法简单,准确,为食品中喹诺酮类药物的残留检测提供了一种有效的分析方法. 相似文献
18.
采用了用高效液相色谱-二极管阵列法测定蜜饯中的5种合成着色剂.用SymmetryC18柱,甲醇-乙酸铵溶液（0.02mol/L）为流动相,流速1.0mL/min,二极管阵列检测器选择柠檬黄428nm、苋菜红520nm、胭脂红510nm、日落黄485nm、亮蓝629nm波长进行检测,并以保留时间和光谱图定性,同时比较了不同前处理方式对测定结果的影响.不同样品的加标回收率为85%～92%. 相似文献
19.
Determination of benzalkonium chloride in viscous ophthalmic drops of azithromycin by high-performance liquid chromatography 总被引：1，自引：0，他引：1
Yan Shen Sheng-jie Xu Shi-chun Wang Jia-sheng Tu 《Journal of Zhejiang University. Science. B》2009,10(12):877-882
A high-performance liquid chromatography (HPLC) system was used in the reversed phase mode for the determination of benzalkonium chloride (BKC) in azithromycin viscous ophthalmic drops. A Venusil-XBP(L)-C_(18) (150 mm×4.6 mm, 5 μm) column was used at 50 ℃. The mobile phase consisted of a mixture of methanol-potassium phosphate (16:5, v/v). Two sample preparation methods were compared. The results suggested that, compared with an extraction procedure, a deproteinization procedure was much quicker and more convenient. Using the deproteinization procedure for sample preparation, calibration curves were linear in the range 5.0～50 μg/ml. The within-day and inter-day coefficients of variation were less than 10%. The average recoveries were determined as 96.70%, 98.52%, and 97.96% at concentrations of 10.0, 30.0, and 50.0 μg/ml, respectively. Variability in precision did not exceed 5%. In conclusion, this HPLC method using a simple sample treatment procedure appears suitable for monitoring BKC content in azithromycin viscous ophthalmic drops. 相似文献
20.
采用YWGC18柱(4.6 mm×250 mm,10μm),以甲醇(80 mmol.L-1)-醋酸铵溶液(pH 6.0)(35:65)为流动相,流速为1.0 mL.min-1;检测波长为310 nm,建立了HPLC法测定湖北利川三种石杉属植物(蛇足石杉、皱边石杉、四川石杉)中石杉碱甲含量,以期发掘替代资源。结果显示,三种石杉属植物中均含有石杉碱甲,且四川石杉最多,蛇足石杉次之,皱边石杉最少,故四川石杉可以作为提取石杉碱甲的原料药材之一,具有较高的开发和利用价值。 相似文献