为准确测定蜂王浆中挥发性化合物的含量,对顶空固相微萃取(headspace-solid phase microextraction,HS-SPME)的萃取温度、萃取时间、样品量、饱和NaCl溶液的添加量在单因素试验的基础上,通过响应面设计进行了萃取条件的优化;依据优化的萃取条件,采用气相色谱-质谱联用(gas chromatography-mass spectrometry,GC-MS)测定了5种不同来源蜂王浆中的挥发性化合物。结果表明,萃取温度62 ℃、萃取时间60 min、蜂王浆2 g、饱和NaCl溶液添加量为1 mL时,总峰面积最大,萃取效果好。5种不同来源蜂王浆共检出了48种挥发性化合物,其中共有的化合物有16种,多为酸、酯和醛类等化合物,但其含量不同,这些共有化合物可能与蜂王浆的特征风味有关。研究结果为蜂王浆挥发性化合物检测和应用提供了参考。
A headspace (HS)/solid phase microextraction (SPME)/gas chromatography-mass spectrometry (GC-MS) method was developed to accurately determine the profiles of volatile compounds from royal jelly based on the single-factor tests of extraction temperature and time, sample size, saturated NaCl solution addition. The optimization of the extraction conditions was carried out by response surface methodology. According to optimized extraction conditions, volatile compounds in royal jelly from five different sources were determined by gas chromatography-mass spectrometry (GC-MS). The analytical conditions of the optimized HS-SPME method were: extraction temperature 62 ℃, extraction time 60 min, 2 g royal jelly, 1 mL saturated NaCl solution. Under this extraction condition, the total peak area was the largest. The GC-MS analysis allowed the identification of 48 volatile compounds in five royal jelly. The 16 common volatile compounds in the samples were rich in acid, ester and aldehyde compounds, but their content was varied. These common compounds may be related to the characteristic flavor of royal jelly. The results could be used for the detection and application of volatile compounds in royal jelly.
[1] LIU J R, YUAN Y C, SHI L S, et al. Antioxidant properties of royal jelly associated with larval age and time of harvest[J].Agric Food Chem. 2008,56 (23): 11 447-11 452.
[2] SCARSELLI R,DONADIO E,GIUFFRIDA M G. Towards royal jelly proteome[J]. Proteomics, 2005,5: 769-776.
[3] ANKLAM E, RADOVIC B.Suitable analytical methods for determining the origin of European honey[J]. American Laboratory, 2001,33: 60-62.
[4] WALDMAR,WARDENLKL,MAGDLENA,et al. A review of theoretical and practical aspects of solid-phase microextraction in food analysis[J]. Institute of Food Science Techology, 2004,39:703-717.
[5] ISIDOROV V A, BAKIER S, GRZECH I. Gas chromatographic-mass spectrometric investigation of volatile and extractable compounds of crude royal jelly[J]. Journal of Chromatography B, 2012, 885:109-116.
[6] ZHAO Y Z, LI Z G, TIAN W L, et al.Differential volatile organic compounds in royal jelly associated with different nectar plants[J].Journal of Integrative Agriculture,2016,15(5):1 157-1 165.
[7] BOSELLI E, CABONI M F, SABATINI A G, et al. Determination and changes of free amino acids in royal jelly during storage[J]. Apidologie, 2003,34(2): 129-138.
[8] 任佳淼,彭文君,田文礼,等.加工工艺对蜂蜜挥发性成分的影响[J].食品科学,2014,35(10):41-45.
[9] CEBALLOS LIENA,PINO JORGE A, DAGO ANGEL, et al. Optimization of a HS-SPME/GC-MS method for determination of volatile compounds in some cuban unifloral honeys[J]. Food Quality,2010, 33(4):507-528.
[10] MIRHOSSEINI H, SALMAH Y, NAZIMAH S A H, et al.Solid-phase microextraction for headspace analysis of key volatile compounds in orange beverage emulsion[J]. Food Chemistry,2007,105: 1 659-1 670.
[11] ZHANG Y, GAO B, ZHANG M, et al. Headspace solid-phase microextraction-gas chromatography-mass spectrometry analysis of the volatile components of longan (Dimocarpus longan Lour.)[J]. Eurpean Food Research and Technology,2009,229:457-465.
[12] KING A J, READMAN J W, ZHOU J L, The application of solid-phase micro-extraction (SPME) to the analysis of polycyclic aromatic hydrocarbons (PAHs)[J]. Environ Geochem Health,2003, 25:69-75.
[13] MOREIRA N, MEIRELES S, BRANDÃO T,et al. Optimization of the HS-SPME-GC-IT/MS method using a central composite design for volatile carbonyl compounds determination in beers[J]. Talanta,2013, 117: 523-531.
[14] BALASUBRAMANIAN S, PANIGRAHI S, Solid-phase microextraction (SPME) techniques for quality characterization of food products: a review[J]. Food Bioprocess Technology,2011,4:1-26.
[15] BARONI M V, NORES M L, DIAZ M D P, et al. Determination of volatile organic compound patterns characteristics of five unifloral honeys by solid-phase microextraction-gas chromatography-mass spectrometry coupled to chemimetrics[J]. Journal of Agricultural and Food Chemistry, 2006,54(19): 7 235-7 241.
[16] MANYI-LOH C E, NDIP R N, CLARKE A M. Volatile compounds in honey: A review on their involvement in aroma, botanical origin determination and potential biomedical activities[J]. International Journal of Molecular Sciences,2011,12(12), 9 514-9 532.
