奥利司他中间体利普司他汀标准品的制备工艺研究
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摘要
目的本文主要发明了一种利普司他汀对照标准品的制备工艺。方法本法先采用了DAC50 C_8制备柱(50mm×450mm,5μm),以86%甲醇-RO水溶液为流动相,上柱液浓度21000μg·mL~(-1),进样量1.4g·L~(-1),检测波长195nm,上柱流速为35mL·min~(-1),洗脱流速为50mL·min~(-1),得到了组分含量超过93%的收集液。再将收集液加入庚烷萃取,后在庚烷相中加入乙腈萃取至乙腈相,减压浓缩。结果得到纯度93%相对含量为85%的利普司他汀标准品。结论本工艺可制备得到可应用于利普司他汀检测的合格标准品。
OBJECTIVE The present invention provides a method for preparing(purifying)standard products of Lipstatin.METHODS The separation was performed on DAC50 C_8 column(50 mm×450 mm,5μm).The mobile phase was 86% methanol-water solution,the injection volume(sample load) was 1.4 g·L~(-1),and detection wavelength was 195 nm,load sample flow was 35 mL·min~(-1),elution flow was 50 mL·min~(-1),the composition of collected sample was over 93%.The collected sample was extracted with heptane,and separated by partitioning.Then add acetonitrile in the heptane solution.RESULTS The aceronitrile solution was concentrated by reducing pressure,concentrate of Lipstatin was obtained.CONCLUSION This method can prepare the standard products of Lipstatin.
OBJECTIVE The present invention provides a method for preparing(purifying)standard products of Lipstatin.METHODS The separation was performed on DAC50 C_8 column(50 mm×450 mm,5μm).The mobile phase was 86% methanol-water solution,the injection volume(sample load) was 1.4 g·L~(-1),and detection wavelength was 195 nm,load sample flow was 35 mL·min~(-1),elution flow was 50 mL·min~(-1),the composition of collected sample was over 93%.The collected sample was extracted with heptane,and separated by partitioning.Then add acetonitrile in the heptane solution.RESULTS The aceronitrile solution was concentrated by reducing pressure,concentrate of Lipstatin was obtained.CONCLUSION This method can prepare the standard products of Lipstatin.
引文
[1]朱美容,许勇煌,王德刚.RP-HPLC测定利普司他汀的含量[P].中国:1673-4610(2013)11-0720-03.
[2]许勇煌,彭韪,唐彬喜,等.一种奥利司他的制备方法[P].中国:201110047178,8,2011-02-28.
[3]赵德,岳光,易昆,等.一种利普司他汀的提纯方法[P].中国:CN,6,2014.
[4]李玲,王艳,张征林.大孔树脂分离纯化利普司他汀[J].《化工时刊》,2013,27(2):25-28.
[5]胡为民,庄英萍,王永红.毒三链霉菌生产利普司他汀的发酵和提取工艺[J].中国医药工业杂志,2007,38(10):705-708.
[2]许勇煌,彭韪,唐彬喜,等.一种奥利司他的制备方法[P].中国:201110047178,8,2011-02-28.
[3]赵德,岳光,易昆,等.一种利普司他汀的提纯方法[P].中国:CN,6,2014.
[4]李玲,王艳,张征林.大孔树脂分离纯化利普司他汀[J].《化工时刊》,2013,27(2):25-28.
[5]胡为民,庄英萍,王永红.毒三链霉菌生产利普司他汀的发酵和提取工艺[J].中国医药工业杂志,2007,38(10):705-708.