高效液相色譜法拆分佐匹克隆對(duì)映體

制藥工程論文編號(hào):ZY096    論文字?jǐn)?shù):10090,頁(yè)數(shù):21

目  錄
中文摘要 …………………………………………………………………………………Ⅰ
英文摘要 …………………………………………………………………………………Ⅱ
目錄 ………………………………………………………………………………………Ⅲ
1. 緒論 ……………………………………………………………………………………1
 1.1前言………………………………………………………………………………1
 1.2佐匹克隆簡(jiǎn)介……………………………………………………………………1
 1.3佐匹克隆對(duì)映體拆分文獻(xiàn)綜述…………………………………………………2
2. 實(shí)驗(yàn)部分 ………………………………………………………………………………6
 2.1 儀器和試劑  ……………………………………………………………………6
 2.2 實(shí)驗(yàn)試劑配制……………………………………………………………………6
     2.2.1 緩沖溶液配制……………………………………………………………6
     2.2.2 流動(dòng)相配制………………………………………………………………6
     2.2.3 對(duì)照品溶液配制…………………………………………………………6
     2.2.4 樣品溶液配制……………………………………………………………7
 2.3 實(shí)驗(yàn)方法…………………………………………………………………………7
     2.3.1 不同色譜條件下分離情況的考察………………………………………7
     2.3.2 線性試驗(yàn)…………………………………………………………………7
 2.3.3 精密度試驗(yàn)………………………………………………………………7
 2.3.4 重復(fù)性試驗(yàn)………………………………………………………………7
 2.3.5 回收率試驗(yàn)………………………………………………………………7
 2.3.6 溶液穩(wěn)定性試驗(yàn)…………………………………………………………7
 2.3.7 樣品含量測(cè)定……………………………………………………………7
3. 結(jié)果與討論 ……………………………………………………………………………8
 3.1 流動(dòng)相組成對(duì)分離的影響………………………………………………………8
 3.2 乙腈體積分?jǐn)?shù)對(duì)分離的影響……………………………………………………8
 3.3 柱溫對(duì)分離的影響………………………………………………………………9
 3.4 流速對(duì)分離的影響………………………………………………………………9
 3.5 流動(dòng)相pH值對(duì)分離的影響……………………………………………………10
 3.6 最佳色譜條件的確立 …………………………………………………………10
 3.7 線性試驗(yàn)結(jié)果 …………………………………………………………………11
 3.8 精密度試驗(yàn)結(jié)果 ………………………………………………………………12
 3.9 重復(fù)性試驗(yàn)結(jié)果 ………………………………………………………………12
 3.10 回收率試驗(yàn)結(jié)果………………………………………………………………13
 3.11 溶液穩(wěn)定性試驗(yàn)結(jié)果…………………………………………………………14
 3.12 含量測(cè)定結(jié)果…………………………………………………………………14
4. 總結(jié)與展望……………………………………………………………………………15
致謝 ………………………………………………………………………………………16
參考文獻(xiàn) …………………………………………………………………………………17

摘 要：本文建立了佐匹克隆（ZPC）對(duì)映體的反相高效液相色譜拆分方法。使用Chiralcel OD-RH(150 mm×4.6mm，5μm)手性柱分離佐匹克隆對(duì)映體，考查了不同流動(dòng)相組分、流動(dòng)相中乙腈含量、pH值、柱溫和流速對(duì)手性拆分結(jié)果的影響。確立測(cè)定的最佳色譜條件為：流動(dòng)相為乙腈-磷酸二氫鉀緩沖液(pH=6.0，V：V=35：65)；流速1.0 mL/min；檢測(cè)波長(zhǎng)為303nm；柱溫30℃。結(jié)果表明佐匹克隆在0.5-8μg/mL之間呈良好線性關(guān)系，線性相關(guān)系數(shù)R/S-ZPC： r＝1，平均回收率R/S-ZPC分別為98.23%，RSD＝0.48%（n＝9）和99.19%，RSD＝0.52%（n＝9），溶液在24h內(nèi)穩(wěn)定。本法操作簡(jiǎn)便、易行、準(zhǔn)確、重復(fù)性好。

關(guān)鍵詞：佐匹克隆；拆分；高效液相色譜法

Abstracts: This article develop an RP-HPLC method to separate zopiclone(ZPC) enantiomers. A Chiralcel OD-RH (150mm×4.6mm，5μm) chiral column was used to separate zopiclone enantiomers．The influence of the different mobile phase，the CH3CN content，the pH Value，the column temperature and the velocity of flow on chiral separation were studied. The best analytic condition was: the mobile phase was composed of acetonitrile and potassium dihydrogen phosphate (pH=6.0, V：V=35：65) and the flow rate was 1.0 mL/min, the detection wavelength was set at 303nm and the column temperature was 30℃. The rusults showed that the linear rang of zopiclone was 0.5-8μg/mL，the linear correlation of R/ S-ZPC was1，The average recoveries of R/S-ZPC were 98.23% and 99.19%, respectively, with RSD of 0.48% and 0.52% (n=9). The solution was steady within 24h. This method is simple, accurate and with good reproducibility.
Key words: Zopiclone; Separation; High Performance Liquid Chromatography