反相高效液相色谱法分离分析花青醛和巴豆醛
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摘要
建立了花青醛和巴豆醛的反相高效液相色谱分离分析方法。考察了缓冲盐的种类、浓度和pH等色谱条件对分离分析的影响。以甲醇-15 mmol/L磷酸二氢钠(pH 6.5)为流动相,在C18色谱柱上,采用梯度洗脱,花青醛和巴豆醛的分析时间在6 min内。花青醛和巴豆醛分别在0.4～1 500μg/mL和0.2～1 500μg/mL范围内线性关系良好(r~2≥0.9971),检出限(信噪比为3)分别为100 ng/mL和50 ng/mL;样品的加标回收率为98.0%～100.2%,相对标准偏差为0.5%～1.4%。该方法操作简单、快速、准确可靠,用于实际样品的分析时,获得了令人满意的结果。
A method for determining the anthocyanic aldehyde and crotonaldehyde by reversed-phase high performance liquid chromatography(RP-HPLC)was developed. The effects of type, concentration and pH of buffer salt on analytical results were investigated. Anthocyanic aldehyde and crotonaldehyde were separated within 6 min using 15 mmol/mL phosphate(pH 6.5)and methanol as mobile phase with a gradient elution program on the C18 column. The calibration curves of anthocyanic aldehyde and crotonaldehyde showed good linearity in the range of 0.4-1 500 μg/mL and 0.2-1 500 μg/mL with correlation coef?cients(r~2)≥ 0.9971, respectively. The limits of detection were 100 ng/mL and 50 ng/mL(S/N=3).The recoveries ranged from 98.0% to 100.2% with acceptable relative standard deviation of 0.5%-1.4%. The method is simple, fast, accurate and reliable. It was successfully used for determining the anthocyanic aldehyde and crotonaldehyde in real samples, and the assay results were satisfactory.
A method for determining the anthocyanic aldehyde and crotonaldehyde by reversed-phase high performance liquid chromatography(RP-HPLC)was developed. The effects of type, concentration and pH of buffer salt on analytical results were investigated. Anthocyanic aldehyde and crotonaldehyde were separated within 6 min using 15 mmol/mL phosphate(pH 6.5)and methanol as mobile phase with a gradient elution program on the C18 column. The calibration curves of anthocyanic aldehyde and crotonaldehyde showed good linearity in the range of 0.4-1 500 μg/mL and 0.2-1 500 μg/mL with correlation coef?cients(r~2)≥ 0.9971, respectively. The limits of detection were 100 ng/mL and 50 ng/mL(S/N=3).The recoveries ranged from 98.0% to 100.2% with acceptable relative standard deviation of 0.5%-1.4%. The method is simple, fast, accurate and reliable. It was successfully used for determining the anthocyanic aldehyde and crotonaldehyde in real samples, and the assay results were satisfactory.
引文
[1]刘树文.合成香料技术手册[M].北京:中国轻工业出版社,2009:154.
[2]ABATE A,BRENNA E,NEGRI C D,et al.Biocatalysed synthesis of the enantiomers of the floral odorant florhydral[J].Tetrahedron Asymmetry,2002,13(8):899-904.
[3]BOVO S,SCRIVANTI A,BERTOLDINI M,et al.A new enantioselective catalytic route to florhydral[J].Synthesis,2008,40(16):2547-2550.
[4]PAGANELLI S,CIAPPA A,MARCHETTI M,et al.Hydroformylation of m-diisopropenylbenzene and 1-isopropyl-3-isopropenyl benzene for the preparation of the fragrance Florhydral[J].Journal of Molecular Catalysis A-Chemical,2006,247(1):138-144.
[5]STADLER M,LIST B.Heck reactions of crotonaldehyde[J].Synlett,2008(4):597-599.
[6]GREMAUD L,ALEXAKIS A.Enantioselective coppercatalyzed conjugate addition of trimethylalu minium toβ,γ-unsaturatedα-ketoesters[J].Angewandte Chemie,2012,51(3):794-797.
[7]GONCALVES-CONTAL S,GREMAUD L,PALAIS L,et al.Coppe-Catalyzed enantioselective conjugate addition toα,β-Unsaturated aldehydes with various organometallic reagents[J].Synthesis,2016,48(19):3301-3308.
[8]DRISSI-AMRAOUI S,SCHMID T E,LAUBERTEAUX J,et al.Copper-Catalyzed asymmetric conjugate addition of dimethylzinc to acyl-N-methylimidazole michael acceptors:scope,limitations and iterative reactions[J].Advanced Synthesis&Catalysis,2016,358(15):2519-2540.
[9]LI J J.有机人名反应及机理[M].荣国斌,译.上海:华东理工大学出版社,2003:253.
[10]HOFLING S B,HULTSCH C,WESTER H,et al.Radiochemical 18F-fluoroarylation of unsaturatedα-,β-andγ-amino acids,application to a radiolabelled analogue of baclofen[J].Tetrahedron,2008,64(52):11846-11851.
[11]YANG Z,CHEN Z,AN Y,et al.Selective and tunable synthesis of 3-arylsuccinimides and 3-arylmaleimides from arenediazonium tetrafluoroborates and maleimides[J].RSCAdvances,2016,47(28):23438-23447.
[2]ABATE A,BRENNA E,NEGRI C D,et al.Biocatalysed synthesis of the enantiomers of the floral odorant florhydral[J].Tetrahedron Asymmetry,2002,13(8):899-904.
[3]BOVO S,SCRIVANTI A,BERTOLDINI M,et al.A new enantioselective catalytic route to florhydral[J].Synthesis,2008,40(16):2547-2550.
[4]PAGANELLI S,CIAPPA A,MARCHETTI M,et al.Hydroformylation of m-diisopropenylbenzene and 1-isopropyl-3-isopropenyl benzene for the preparation of the fragrance Florhydral[J].Journal of Molecular Catalysis A-Chemical,2006,247(1):138-144.
[5]STADLER M,LIST B.Heck reactions of crotonaldehyde[J].Synlett,2008(4):597-599.
[6]GREMAUD L,ALEXAKIS A.Enantioselective coppercatalyzed conjugate addition of trimethylalu minium toβ,γ-unsaturatedα-ketoesters[J].Angewandte Chemie,2012,51(3):794-797.
[7]GONCALVES-CONTAL S,GREMAUD L,PALAIS L,et al.Coppe-Catalyzed enantioselective conjugate addition toα,β-Unsaturated aldehydes with various organometallic reagents[J].Synthesis,2016,48(19):3301-3308.
[8]DRISSI-AMRAOUI S,SCHMID T E,LAUBERTEAUX J,et al.Copper-Catalyzed asymmetric conjugate addition of dimethylzinc to acyl-N-methylimidazole michael acceptors:scope,limitations and iterative reactions[J].Advanced Synthesis&Catalysis,2016,358(15):2519-2540.
[9]LI J J.有机人名反应及机理[M].荣国斌,译.上海:华东理工大学出版社,2003:253.
[10]HOFLING S B,HULTSCH C,WESTER H,et al.Radiochemical 18F-fluoroarylation of unsaturatedα-,β-andγ-amino acids,application to a radiolabelled analogue of baclofen[J].Tetrahedron,2008,64(52):11846-11851.
[11]YANG Z,CHEN Z,AN Y,et al.Selective and tunable synthesis of 3-arylsuccinimides and 3-arylmaleimides from arenediazonium tetrafluoroborates and maleimides[J].RSCAdvances,2016,47(28):23438-23447.