高效液相色谱法同时测定那格列奈中顺式异构体和L-异构体
Simultaneous Determination of the Cis-Isomer and L-Isomer in Nateglinide by HPLC
摘 要
称取样品25 mg，用正己烷-无水乙醇-三氟乙酸（80+20+0.1）混合溶液溶解并定容至25 mL，采用Chiralpak IG色谱柱（250 mm×4.6 mm，5 μm）分离待测物，以正己烷-无水乙醇-三氟乙酸（80+20+0.1）混合溶液为流动相，流量为0.8 mL·min-1，采用二极管阵列检测器进行测定，检测波长为210 nm。那格列奈的顺式异构体和L-异构体的质量浓度分别在0.024~4.392，0.050~4.040 mg·L-1内与其峰面积呈线性关系，检出限（3S/N）分别为0.008，0.015 mg·L-1。加标回收率分别在94.1%~99.3%，100%~104%之间，测定值的相对标准偏差（n=6）小于5.0%。
那格列奈
顺式异构体
L-异构体
HPLC
nateglinide
cis-isomer
L-isomer
Abstract
The sample (25 mg) was dissolved and the solution was diluted to 25 mL with a mixed solution of hexane-ethanol-trifluoroacetate (80+20+0.1). Chromatographic separation was achieved on a Chiralpak IG column (250 mm×4.6 mm, 5 μm), with a mixed solution of hexane-ethanol-trifluoroacetate (80+20+0.1) as mobile phase, at a fow rate of 0.8 mL·min-1. Diode array detector was used for determination at wavelength of 210 nm. Linear relationships were found between peak areas and mass concentraions of cis-isomer and L-isomer in the ranges of 0.024-4.392, 0.050-4.040 mg·L-1, respectively, with detecion limits (3S/N) of 0.008, 0.015 mg·L-1 respectively. Values of recovery obtained by standard additon method were in the range of 94.1%-99.3%, 100%-104%, respectively, and RSDs (n=6) were less than 5.0%.
中图分类号 O657.7 DOI 10.11973/lhjy-hx201803017
所属栏目 工作简报
基金项目
收稿日期 2017/3/3
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备注董淑波(1984-),男,江苏连云港人,博士研究生,主要从事新药研发工作,456shu@163.com
引用该论文: DONG Shubo,YANG Hanyue,CHEN Xuemin,YE Deju. Simultaneous Determination of the Cis-Isomer and L-Isomer in Nateglinide by HPLC[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(3): 326～330
董淑波,杨汉跃,陈学民,叶德举. 高效液相色谱法同时测定那格列奈中顺式异构体和L-异构体[J]. 理化检验－化学分册, 2018, 54(3): 326～330
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参考文献
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【4】PHAN T D, NGUYEN N H, KIM D J, et al. Determination of the L-enantiomer of nateglinide in pharmaceutical formulations by micellar electrokinetic chromatography[J]. Archires of Pharmacal Research, 2010,33(12):2017-2024.
【5】Committee of Revision. USP36-NF31[M]. Rockville:The United States Pharmacopeia Convention, 2013.
【6】YANG G, LI Z, WANG D, et al. Chiral separation of N-(trans-4-isopropylcyclohexylcarbonyl)-D, L-phenylalanine isomers by high performance liquid chromatography[J]. Chromatographia, 2002,56(7/8):515-518.
【7】YANG G, YIN J, LI Z, et al. Chiral separation of nateglinide and its L-enantiomer on a molecularly imprinted polymer-based stationary phase[J]. Chromatographia, 2004,59(11/12):705-708.
【8】SANGARAJU S, RAO B M, SRINIVAS T, et al. A validated chiral LC method for the enantiomeric separation of nateglinide and the quantitative determination of its L-enantiomer[J]. Chromatographia, 2009,69(9/10):1123-1127.
【9】李语如,韦艳丽,顾萍,等.那格列奈中L-异构体和顺式异构体的HPLC法测定[J].药物分析杂志, 2006,26(4):443-445.
【10】SANKALIA J M, SANKALIA M G, SUTARIYA V B, et al. Nateglinide quantification in rabbit plasma by HPLC:Optimization and application to pharmacokinetic study[J]. Journal of Pharmaceutial and Biomedical Analysis, 2007,44(1):196-204.
【2】PRASHANT A N, SHARMA J C, POTNURI N, et al. Formulation and evaluation of oral disintegrating tablets of nateglinide[J]. Der Pharmacia Lettre, 2015,7(2):49-59.
【3】LI B H, TIAN B J, LV Y K. Simultaneous chiral separation of geometry isomers and enantiomers of nateglinide by capillary electrophoresis with mixture of CD derivations as chiral selector[J]. Analytical Letters, 2008,41(17):3177-3186.
【4】PHAN T D, NGUYEN N H, KIM D J, et al. Determination of the L-enantiomer of nateglinide in pharmaceutical formulations by micellar electrokinetic chromatography[J]. Archires of Pharmacal Research, 2010,33(12):2017-2024.
【5】Committee of Revision. USP36-NF31[M]. Rockville:The United States Pharmacopeia Convention, 2013.
【6】YANG G, LI Z, WANG D, et al. Chiral separation of N-(trans-4-isopropylcyclohexylcarbonyl)-D, L-phenylalanine isomers by high performance liquid chromatography[J]. Chromatographia, 2002,56(7/8):515-518.
【7】YANG G, YIN J, LI Z, et al. Chiral separation of nateglinide and its L-enantiomer on a molecularly imprinted polymer-based stationary phase[J]. Chromatographia, 2004,59(11/12):705-708.
【8】SANGARAJU S, RAO B M, SRINIVAS T, et al. A validated chiral LC method for the enantiomeric separation of nateglinide and the quantitative determination of its L-enantiomer[J]. Chromatographia, 2009,69(9/10):1123-1127.
【9】李语如,韦艳丽,顾萍,等.那格列奈中L-异构体和顺式异构体的HPLC法测定[J].药物分析杂志, 2006,26(4):443-445.
【10】SANKALIA J M, SANKALIA M G, SUTARIYA V B, et al. Nateglinide quantification in rabbit plasma by HPLC:Optimization and application to pharmacokinetic study[J]. Journal of Pharmaceutial and Biomedical Analysis, 2007,44(1):196-204.
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