建立了一种快速、准确的高效液相色谱分析方法。使用Chiralpak AD-H手性色谱柱,检测波长224nm,考察了流动相中极性调节剂的体积分数、流动相中三乙胺的体积分数、柱温及流速对西那卡塞对映体拆分的影响。确立了最佳拆分条件:流动相为正...建立了一种快速、准确的高效液相色谱分析方法。使用Chiralpak AD-H手性色谱柱,检测波长224nm,考察了流动相中极性调节剂的体积分数、流动相中三乙胺的体积分数、柱温及流速对西那卡塞对映体拆分的影响。确立了最佳拆分条件:流动相为正己烷-异丙醇-三乙胺(90∶10∶0.1,V/V/V);流速为1.0 m L·min-1;柱温为30℃。在此优化实验条件下,得到西那卡塞对映体的出峰顺序为:先S体,后R体。所建立的方法简单准确,重复性好,可用于西那卡塞的质量研究和控制。展开更多
目的建立简便、灵敏的手性高效液相色谱法检查苄基依折麦布中的异构体杂质。方法以Chiralpak IC为固定相,正己烷-异丙醇（体积比90∶10）为流动相,流速为1.0 m L·min-1,检测波长为232 nm。结果通过对分离条件进行优化,苄基依折麦...目的建立简便、灵敏的手性高效液相色谱法检查苄基依折麦布中的异构体杂质。方法以Chiralpak IC为固定相,正己烷-异丙醇（体积比90∶10）为流动相,流速为1.0 m L·min-1,检测波长为232 nm。结果通过对分离条件进行优化,苄基依折麦布与其异构体杂质能达到良好分离。苄基依折麦布在质量浓度为1.0～12 mg·L-1内线性关系良好。平均回收率为99.8%,日内与日间精密度均小于3.0%。结论所建立的分析方法灵敏度高、重现性好,适用于苄基依折麦布中异构体杂质的检查。展开更多
Recent reports have demonstrated that the new commercially available immobilized-type chiral stationary phases（CSPs） containing amylose tris（3-chloro-5-methylphenylcarbamate）（ACMPC） as a selector exhibit not onl...Recent reports have demonstrated that the new commercially available immobilized-type chiral stationary phases（CSPs） containing amylose tris（3-chloro-5-methylphenylcarbamate）（ACMPC） as a selector exhibit not only an exceptionally high enantioselectivity in high-performance liquid chromatography（HPLC） but they are also applicable to a wide range of chiral analytes. Herein, we report the results obtained in the HPLC analysis of omeprazole and its impurities B and E on the ACMPC-based Chiralpak IG-3 CSP（CSP） under polar organic conditions. A systematic evaluation of the retention characteristics of the selected benzimidazole chiral probes was carried out by changing the composition of the mobile phase and the column temperature. It is worth emphasizing that the high affinity of both enantiomers of all analytes recorded in pure methanol mode dramatically decreased incorporating small volumes of either basic or acid additives in the mobile phase. Unspecified sites of the IG-3 CSP presumably involved in strong and non-stereoselective H-bonding contacts with chiral analytes are assumed responsible for the unproductive retention process.展开更多
A simple analytical high-performance liquid chromatography （HPLC） method was applied for the en- antiomeric excess determination of esomeprazole （（S）-OME）, the enantiopure active ingredient con- tained in drug p...A simple analytical high-performance liquid chromatography （HPLC） method was applied for the en- antiomeric excess determination of esomeprazole （（S）-OME）, the enantiopure active ingredient con- tained in drug products, in the presence of its potential organic impurities A-E. The enantioselective separation was accomplished on the immobilized-type Chiralpak ID-3 chiral stationary phase （CSP） under reversed-phase conditions. The results were evaluated and compared with those obtained by the official enantioselective method of European Pharmacopoeia used as the reference for checking the enantiomeric excess of （S）-OME. It has been established that the use of the Chiralpak ID-3 CSP allows the determination of the enantiomeric purity of （S）-OME without any interference coming from its chiral and achiral related substances. The analytical procedure of the drug regulatory agencies based on the AGP CSP suffered instead from poor specificity due to overlap of the peaks pertinent to the achiral impurity A and the chiral impurity （R）-OME （impurity F）.展开更多
文摘建立了一种快速、准确的高效液相色谱分析方法。使用Chiralpak AD-H手性色谱柱,检测波长224nm,考察了流动相中极性调节剂的体积分数、流动相中三乙胺的体积分数、柱温及流速对西那卡塞对映体拆分的影响。确立了最佳拆分条件:流动相为正己烷-异丙醇-三乙胺(90∶10∶0.1,V/V/V);流速为1.0 m L·min-1;柱温为30℃。在此优化实验条件下,得到西那卡塞对映体的出峰顺序为:先S体,后R体。所建立的方法简单准确,重复性好,可用于西那卡塞的质量研究和控制。
基金funding from the European Community's Seventh Framework Programme under the grant agreement 602051 (Project HERACLES: Humancystic Echinococcosis Rese Arch in Centra L and Eastern Societies http://www.Heracles-fp7.eu/)
文摘Recent reports have demonstrated that the new commercially available immobilized-type chiral stationary phases（CSPs） containing amylose tris（3-chloro-5-methylphenylcarbamate）（ACMPC） as a selector exhibit not only an exceptionally high enantioselectivity in high-performance liquid chromatography（HPLC） but they are also applicable to a wide range of chiral analytes. Herein, we report the results obtained in the HPLC analysis of omeprazole and its impurities B and E on the ACMPC-based Chiralpak IG-3 CSP（CSP） under polar organic conditions. A systematic evaluation of the retention characteristics of the selected benzimidazole chiral probes was carried out by changing the composition of the mobile phase and the column temperature. It is worth emphasizing that the high affinity of both enantiomers of all analytes recorded in pure methanol mode dramatically decreased incorporating small volumes of either basic or acid additives in the mobile phase. Unspecified sites of the IG-3 CSP presumably involved in strong and non-stereoselective H-bonding contacts with chiral analytes are assumed responsible for the unproductive retention process.
文摘A simple analytical high-performance liquid chromatography （HPLC） method was applied for the en- antiomeric excess determination of esomeprazole （（S）-OME）, the enantiopure active ingredient con- tained in drug products, in the presence of its potential organic impurities A-E. The enantioselective separation was accomplished on the immobilized-type Chiralpak ID-3 chiral stationary phase （CSP） under reversed-phase conditions. The results were evaluated and compared with those obtained by the official enantioselective method of European Pharmacopoeia used as the reference for checking the enantiomeric excess of （S）-OME. It has been established that the use of the Chiralpak ID-3 CSP allows the determination of the enantiomeric purity of （S）-OME without any interference coming from its chiral and achiral related substances. The analytical procedure of the drug regulatory agencies based on the AGP CSP suffered instead from poor specificity due to overlap of the peaks pertinent to the achiral impurity A and the chiral impurity （R）-OME （impurity F）.
