高效液相色谱法测定卡格列净中葡萄糖酸-δ-内酯的含量
HPLC Determination of Glucono-δ-Lactone in Canagliflozin
摘 要
提出了高效液相色谱-电雾式检测器法（HPLC-CAD）测定卡格列净中葡萄糖酸-δ-内酯（GDL）的含量。优化的色谱条件如下：Thermo Hypersil Gold Aq色谱柱（250 mm×4.6 mm，5 μm），流动相为乙腈（9+1）混合溶液，流量0.5 mL·min-1，柱温30 ℃，进样量10 μL；电雾式检测器（CAD）的雾化温度为50 ℃，载气压力427.5 kPa。在上述的色谱条件下，GDL的线性范围为1.05~22.5 mg·L-1，GDL的检出限（3S/N）为0.32 ng。在3个浓度水平上进行加标回收试验，测得回收率在96.2%~103%之间。供试品加标溶液和对照品溶液在室温条件下放置12 h内稳定，测定值的相对标准偏差（n=7）分别为1.8%，1.3%。
电雾式检测器
葡萄糖酸-δ-内酯
卡格列净
HPLC
Charged aerosol detection
Glucono-δ-Lactone
Canagliflozin
Abstract
A method for determination of Glucono-δ-Lactone (GDL) in Canagliflozin was proposed by HPLC coupled with charged aerosol detection (HPLC-CAD). The optimized chromatographic conditions were as follows:① Thermo Hypersil Gold Aq column (250 mm×4.6 mm, 5 μm) was used as stationary phase; ② the mobile phase was a mixture of acetonitrile-water (9+1) solution with a flow rate of 0.5 mL·min-1; ③ column temperature was 30 ℃; ④ the injection volume was 10 μL; ⑤ the nebulization temperature of CAD was set at 50 ℃, and pressure of carrier gas was 427.5 kPa. Under above chromatographic conditions, linearity range for GDL in mass concentration found was 1.05-22.5 mg·L-1, and the detection limit (3S/N) found was 0.32 ng. Test for recovery was made by standard addition method at 3 concentration levels, giving results in the range of 96.2%-103%. The sample solution and reference solution were stable for 12 h at room temperature, and RSDs (n=7) found were 1.8% and 1.3%, respectively.
中图分类号 O652.63 DOI 10.11973/lhjy-hx201704004
所属栏目 试验与研究
基金项目
收稿日期 2016/5/16
修改稿日期
网络出版日期
作者单位点击查看
备注董淑波(1984-),男,江苏连云港人,博士研究生,主要从事药物分析研究工作。
引用该论文: DONG Shu-bo,YANG Han-yue,YAN Zheng-yu. HPLC Determination of Glucono-δ-Lactone in Canagliflozin[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2017, 53(4): 387～392
董淑波,杨汉跃,严拯宇. 高效液相色谱法测定卡格列净中葡萄糖酸-δ-内酯的含量[J]. 理化检验－化学分册, 2017, 53(4): 387～392
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参考文献
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【2】TAKEUCHI K P, CUNHA R L. Influence of ageing time on sodium caseinate gelation induced by glucono-δ-lactone at different temperatures[J]. Dairy Science and Technology, 2008,88(6):667-681.
【3】岳振峰,吴晖.D-葡萄糖酸-δ-内酯在食品工业中的应用[J].食品科技, 1998(6):32-33.
【4】DESAI S J, PARIHAR J A, PATEL J M, et al. Process for preparation and purification of canagliflozin: US 20160002275[P]. 2016-01-07.
【5】MENG W, ELLSWORTH B A, NIRSCHL A A, et al. Discovery of dapagliflozin: a potent, selective renal sodium-dependent glucose cotransporter 2 (SGLT2) inhibitor for the treatment of type 2 diabetes[J]. Journal of Medicinal Chemistry, 2008,51(5):1145-1149.
【6】HRAPCHAK M, LATLI B, WANG X J, et al. Synthesis of empagliflozin, a novel and selective sodium-glucose co-transporter-2 inhibitor, labeled with carbon-14 and carbon-13[J]. Journal of Labelled Compounds and Radiopharmaceuticals, 2014,57(12):687-694.
【7】ACTON J C, DICK R L. Cured pigment and color development in fermented sausage containing glucono-delta-lactone[J]. Journal of Food Protection®, 1977,40(6):398-401.
【8】INS No. 575 Glucono-δ-Lactone (Glucono-Delta-Lactone, Gluconolactone, Delta-Gluconolactone, GDL[S].
【9】陈建文,朱友亮,丁凤兰,等.食品添加剂D-葡萄糖酸-δ-内酯含量的测定方法研究[J].预防医学论坛, 2009(5):434-436.
【10】GB/T 9695.17-2008 肉与肉制品 葡萄糖酸-δ-内酯含量的测定[S].
【11】LAKER M F, MOUNT J N. Mannitol estimation in biological fluids by gas-liquid chromatography of trimethylsilyl derivatives[J]. Clinical Chemistry, 1980,26(3):441-443.
【12】张协光,刘文丽,曾泳艇,等.气相色谱-质谱法测定食品中葡萄糖酸-δ-内酯[J].化学分析计量, 2015,24(3):27-29.
【13】张协光,刘文丽,郑彦婕.高效液相色谱法测定食品中的葡萄糖酸-δ-内酯[J].中国食品添加剂, 2015(9):161-167.
【14】文红,朱宽正.HPLC测定内酯豆腐中葡萄糖酸-δ-内酯[J].中国卫生检验杂志, 2008,18(9):1776-1777.
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【19】GUO S, LIU J, ZHENG Y, et al. Characterization of transcriptome dynamics during watermelon fruit development: sequencing, assembly, annotation and gene expression profiles[J]. BMC Genomics, 2011,12(1):454-466.
【20】NIHIRA T, SUZUKI E, KITAOKA M, et al. Discovery of β-1,4-D-mannosyl-N-acetyl-D-glucosamine phosphorylase involved in the metabolism of N-glycans[J]. Journal of Biological Chemistry, 2013,288(38):27366-27374.
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【22】OKABE H, HUI S P, FUDA H, et al. Mass spectrometric quantification of amphipathic, polyphenolic antioxidant of the pacific oyster (crassostrea gigas)[J]. Analytical Sciences, 2015,31(12):1341-1344.
【23】RATHOD D M, PATEL K R, MISTRI H N, et al. Application of an LC-MS/MS method for reliable determination of amodiaquine, N-desethylamodiaquine, artesunate and dihydroartemisinin in human plasma for a bioequivalence study in healthy Indian subjects[J]. Journal of Pharmaceutical and Biomedical Analysis, 2016,124:67-78.
【24】GRUMBACH E S, DIEHL D M, NEUE U D. The application of novel 1.7 μm ethylene bridged hybrid particles for hydrophilic interaction chromatography[J]. Journal of Separation Science, 2008,31(9):1511-1518.
【25】ITO K. Advantages of Shodex(TM) NH2P series, polymer-based amino HILIC column, over silica-based amino HILIC columns[J]. LC GC North America, 2011:56-56.
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