摘要
以合成的1,3,5,7-四甲基-8-丙酰肼-二氟化硼-二吡咯甲烷(BODIPY-丙酰肼)作为柱前荧光衍生试剂,用于高效液相色谱分离荧光法检测甲醛、乙醛、丙醛、丁醛、戊醛、己醛、庚醛、辛醛、壬醛、癸醛、十一醛、十二醛等12种脂肪醛。通过对衍生条件和分离条件进行优化,建立了测定脂肪醛的HPLC/FD新方法。衍生反应以H3PO4作催化剂,在60℃时试剂与脂肪醛30 min内反应完全,生成稳定的衍生产物。采用C18柱分离衍生产物,以含20%四氢呋喃的乙腈和pH 6.5的HCOOH-NH3.H2O的缓冲溶液为流动相进行梯度洗脱,在λex/λem=490 nm/510 nm下荧光检测,各脂肪醛衍生物在20 min内得到较好的分离(甲、乙醛衍生峰重叠)。测定脂肪醛的线性范围均为0.01～2.00μmol.L-1,检出限为0.23～0.78 nmol.L-1。该方法用于白酒中脂肪醛含量的测定,加标回收率为95%～105%,结果满意。
A new fluorescent labeling reagent, 1, 3, 5, 7-tetramethyl-8-propionohydrazide-difluoroboradiaza-s-indacene （BODIPY-propionohydrazide）, was synthesized for the determination of C1 - C12 aliphatic aldehydes by high performance liquid chromatography（HPLC）. The experimental conditions were optimized. In the presence of phosphorous acid as a catalyst, the derivatization reaction of BODIPY-propionohydrazide with aldehydes was completed in 30 min at 60℃. The stable BODIPY hydrazone derivatives （ except for formaldehyde and acetaldehyde derivatives） could be separated in 20 rain with acetonitrile （containing 20% tetrahydrofuran） and HCOOH -NH3 · H2O as mobile phase （pH = 6.5）. Under the optimal conditions, the calibration curves of CI - Cj2 aliphatic aldehydes were linear in the range of 0. 01 - 2.00 μmol· L- 1 with detection limits （ S/N = 3 ） of 0. 23 - 0. 78 nmol · L-1 The established method was applied in the determination of aliphatic aldehydes in wine samples with spiked recoveries of 95% -105%.
出处
《分析测试学报》
CAS
CSCD
北大核心
2011年第4期401-406,共6页
Journal of Instrumental Analysis
基金
黄冈师范学院博士基金资助项目(10CD001)
黄冈师范学院自然科学基金资助项目(05CA29)
关键词
荧光试剂
1
3
5
7-四甲基-8-丙酰肼-二氟化硼-二吡咯甲烷
脂肪醛
高效液相色谱
白酒
fuorescent labeling reagent
1, 3, 5, 7-tetramethyl-8-propionohydrazide-difluoroboradiaza-s-indacene
aliphatic aldehydes
high performance liquid chromatography
wine
