Zawirska-Wojtasiak Renata, Wasowicz Erwin
Agricultural University of A. Cieszkowski, Poznań, Institute of Food Technology, Wojska Polskiego 31, PL-60-624, Poznań, Poland.
Nahrung. 2002 Oct;46(5):357-9. doi: 10.1002/1521-3803(20020901)46:5<357::AID-FOOD357>3.0.CO;2-W.
Solid-phase microextraction (SPME) was examined for its suitability for isolation of volatiles from seeds of dill in comparison with the traditional steam distillation procedure. Two main dill seeds volatiles, carvone and limonene, were taken into consideration. Two Supelco SPME fibers were used for the extraction: polyacrylic (PAc) and polydimethylsiloxane (PDMS). The time required to saturate the fibers was 3 min, while distillation took 3 h. Gas chromatography (GC) separation was reduced to 5 min by use of microcapillary column HP-5 cross-linked 5% Ph Me Siloxane. The standards of limonene and carvone were used to prepare calibration curves. PAc fiber responses were described by quadratic curves while PDMS responded linearly. Six varieties of dill were examined by distillation and SPME with both fibers. The good results were achieved for carvone by SPME-PDMS with significant regression between distillation and SPME. This compound can be measured in dill seeds samples within 10 min. The SPME-PDMS were also tested for its application to chiral resolution of carvone and limonene enantiomers in dill seeds oil. The enantiomeric separation was done with two chiral columns. The enantiomeric ratios measured by SPME were just the same as with distillation.
与传统的水蒸气蒸馏法相比,研究了固相微萃取(SPME)从莳萝种子中分离挥发物的适用性。考虑了莳萝种子的两种主要挥发物,香芹酮和柠檬烯。使用两种Supelco SPME纤维进行萃取:聚丙烯酸酯(PAc)和聚二甲基硅氧烷(PDMS)。使纤维饱和所需的时间为3分钟,而蒸馏需要3小时。通过使用微毛细管柱HP-5交联5%苯基甲基硅氧烷,气相色谱(GC)分离时间缩短至5分钟。使用柠檬烯和香芹酮标准品绘制校准曲线。PAc纤维的响应呈二次曲线,而PDMS呈线性响应。用两种纤维通过蒸馏和SPME对六个莳萝品种进行了检测。SPME-PDMS对香芹酮取得了良好的结果,蒸馏和SPME之间具有显著的相关性。该化合物可在10分钟内对莳萝种子样品进行测定。还测试了SPME-PDMS在莳萝籽油中香芹酮和柠檬烯对映体手性拆分的应用。使用两根手性柱进行对映体分离。通过SPME测量的对映体比例与蒸馏法相同。