色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2014年
11期
1219-1224
,共6页
程彪平%李来生%周仁丹%聂桂珍%张宏福
程彪平%李來生%週仁丹%聶桂珍%張宏福
정표평%리래생%주인단%섭계진%장굉복
高效液相色谱法%β-环糊精键合 SBA-15 固定相%β-受体阻滞剂%阿替洛尔%对映体含量测定%片剂
高效液相色譜法%β-環糊精鍵閤 SBA-15 固定相%β-受體阻滯劑%阿替洛爾%對映體含量測定%片劑
고효액상색보법%β-배호정건합 SBA-15 고정상%β-수체조체제%아체락이%대영체함량측정%편제
high performance liquid chromatography(HPLC)%β-cyclodextrin-bonded SBA-15 stationary phase(NESP)%β-adrenergic blockers%atenolol%quantification of enantiomers%tablets
以有序介孔材料（ SBA-15）为基质，制备了一种二硝基苯醚化β-环糊精键合 SBA-15液相色谱手性固定相（NESP）。优化了流动相和温度等色谱条件，在极性有机溶剂模式下，采用实验室自制的手性柱，实现了阿替洛尔对映体的快速拆分。优化的流动相组成为乙腈/甲醇/冰醋酸/三乙胺（90：10：2.5：3.0，v / v / v / v），流速为0.5 mL / min，柱温为20℃，检测波长为275 nm。在上述色谱条件下，阿替洛尔对映体的分离度为1.73，分析时间约为20 min。阿替洛尔药片经甲醇提取并直接进样分析，实现了阿替洛尔片剂中对映体含量的测定。阿替洛尔的两对映体的质量浓度在2.5~100 mg / L 范围内呈良好的线性关系（r 分别为0.9992和0.9989）。采用标准添加法测得两对映体在片剂中的回收率为94.60％~97.24％。样品测定结果的日内和日间相对标准偏差（ RSD）分别不大于0.92％和1.86％（n =5）。按3倍信噪比确定出最小检测质量浓度为0.2 mg / L。该方法简便、选择性好、回收率较高，自制环糊精手性柱可降低测试成本，在手性药物的快速质量监测和药代动力学研究中具有良好的应用前景。
以有序介孔材料（ SBA-15）為基質，製備瞭一種二硝基苯醚化β-環糊精鍵閤 SBA-15液相色譜手性固定相（NESP）。優化瞭流動相和溫度等色譜條件，在極性有機溶劑模式下，採用實驗室自製的手性柱，實現瞭阿替洛爾對映體的快速拆分。優化的流動相組成為乙腈/甲醇/冰醋痠/三乙胺（90：10：2.5：3.0，v / v / v / v），流速為0.5 mL / min，柱溫為20℃，檢測波長為275 nm。在上述色譜條件下，阿替洛爾對映體的分離度為1.73，分析時間約為20 min。阿替洛爾藥片經甲醇提取併直接進樣分析，實現瞭阿替洛爾片劑中對映體含量的測定。阿替洛爾的兩對映體的質量濃度在2.5~100 mg / L 範圍內呈良好的線性關繫（r 分彆為0.9992和0.9989）。採用標準添加法測得兩對映體在片劑中的迴收率為94.60％~97.24％。樣品測定結果的日內和日間相對標準偏差（ RSD）分彆不大于0.92％和1.86％（n =5）。按3倍信譟比確定齣最小檢測質量濃度為0.2 mg / L。該方法簡便、選擇性好、迴收率較高，自製環糊精手性柱可降低測試成本，在手性藥物的快速質量鑑測和藥代動力學研究中具有良好的應用前景。
이유서개공재료（ SBA-15）위기질，제비료일충이초기분미화β-배호정건합 SBA-15액상색보수성고정상（NESP）。우화료류동상화온도등색보조건，재겁성유궤용제모식하，채용실험실자제적수성주，실현료아체락이대영체적쾌속탁분。우화적류동상조성위을정/갑순/빙작산/삼을알（90：10：2.5：3.0，v / v / v / v），류속위0.5 mL / min，주온위20℃，검측파장위275 nm。재상술색보조건하，아체락이대영체적분리도위1.73，분석시간약위20 min。아체락이약편경갑순제취병직접진양분석，실현료아체락이편제중대영체함량적측정。아체락이적량대영체적질량농도재2.5~100 mg / L 범위내정량호적선성관계（r 분별위0.9992화0.9989）。채용표준첨가법측득량대영체재편제중적회수솔위94.60％~97.24％。양품측정결과적일내화일간상대표준편차（ RSD）분별불대우0.92％화1.86％（n =5）。안3배신조비학정출최소검측질량농도위0.2 mg / L。해방법간편、선택성호、회수솔교고，자제배호정수성주가강저측시성본，재수성약물적쾌속질량감측화약대동역학연구중구유량호적응용전경。
A novel dinitrophenyl ether β-cyclodextrin-bonded chiral stationary phase( NESP) for HPLC was prepared with ordered mesoporous SBA-15 as matrix. The fast enantioseparation of atenolol enantiomers on the new stationary phase was achieved through the optimization of mobile phase composition,column temperature and other factors in polar organic solvent mode. The optimized composition of mobile phase was acetonitrile / methanol / glacial acetic acid / triethylamine(90 :10 :2. 5 :3. 0,v / v / v / v)at the flow rate of 0. 5 mL / min. The column tem-perature was set at 20 ℃ . The detection wavelength was 275 nm. The resolution of atenolol enantiomers was 1. 73 with a rather short analysis time,about 20 min,under the above condi-tions. The atenolol was extracted with methanol from the tablets and analyzed by direct injec-tion for HPLC. A new quantitative method of atenolol enantiomers in tablets was established after the condition optimization. The good linear relationships for two atenolol enantiomers were observed in the range of 2. 5-100 mg / L with r of 0. 999 2 and 0. 998 9,respectively. The recoveries of atenolol enantiomers in tablet samples were 94. 60% -97. 24% . The relative stand-ard deviations(RSDs)of this method were not greater than 0. 92% for intra-day and 1. 86% for inter-day,respectively. The detection limits( S / N = 3)of concentrations were less than 0. 2 mg / L for both enantiomers. The established method is simple and of high selectivity,high recovery and low cost for enantiomer analysis by using homemade cyclodextrin-based chiral column. It has a good application prospect for the fast quality control and the pharmacokinetics study of chiral drugs.
