食品研究与开发:2025,46(19):169-174
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固相萃取-气相色谱/质谱法测定蜂蜜中正己酸含量及其在米团花蜂蜜鉴别中的应用
郭怀娇1,祖铁红2,李佳琪2,管志斌3,黄学者2,李阿丹1 *,崔宗岩2*
(1.燕山大学 环境与化学工程学院,河北 秦皇岛 066004;2.秦皇岛海关技术中心,河北 秦皇岛 066004;3.西双版纳金棕生物科技有限公司,云南 景洪 666100)
Determination of Hexanoic Acid Content in Honey by Solid Phase Extraction-Gas Chromatography/Mass Spectrometry and Its Application in Identification of Leucosceptrum canum Smith Honey
GUO Huaijiao1,ZU Tiehong2,LI Jiaqi2,GUAN Zhibin3,HUANG Xuezhe2,LI Adan1*,CUI Zongyan2*
(1.College of Environmental and Chemical Engineering,Yanshan University,Qinhuangdao 066004,Hebei,China;2.Technology Center of Qinhuangdao Customs,Qinhuangdao 066004,Hebei,China;3.Xishuangbanna Jinzong Biotechnology Co.,Ltd.,Jinghong 666100,Yunnan,China)
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投稿时间:2024-09-02    
中文摘要: 为建立一种固相萃取-气相色谱/质谱(solid phase extraction-gas chromatography-mass spectrometry,SPE-GC/MS)测定蜂蜜中正己酸含量的方法,蜂蜜样品经去离子水溶解后,调节pH值为8.0±0.5,采用Strata-X-A固相萃取柱对正己酸进行富集净化,2%甲酸-甲醇洗脱,氮吹后用2 mL 50%甲醇水溶液复溶,采用GC-MS对正己酸进行测定。结果表明,正己酸在0.1~10 mg/L浓度范围内线性关系良好(R2=0.999 8)。方法检出限为0.06 mg/kg,定量限为0.20 mg/kg。在空白样品中进行0.2、0.4、2.0 mg/kg 3个浓度水平的添加测试,回收率为96.8%~107.6%,相对标准偏差为0.8%~4.1%(n=6)。采用该方法对16批米团花蜂蜜和61批其他蜜种蜂蜜进行检测,发现其他蜂蜜中均未检出正己酸,而米团花蜂蜜中全部检出正己酸,其含量范围为0.30~4.14 mg/kg。因此该方法操作简便、灵敏度高、准确性好,适用于蜂蜜中正己酸含量的测定,同时正己酸可以作为米团花蜂蜜的潜在特征成分,用于其真实性鉴别与品质评价。
Abstract:To establish a method for determining hexanoic acid content in honey by solid phase extraction-gas chromatography/mass spectrometry(SPE-GC/MS),honey samples were dissolved in deionized water,and the pH was adjusted to 8.0±0.5.The Strata-X-A solid-phase extraction column was used to enrich and purify hexanoic acid.The sample solution was eluted with a 2% formic acid-methanol solution,dried under a nitrogen stream,and redissolved with 2 mL of 50% methanol-water solution.Finally,hexanoic acid was determined by GC-MS.The results showed that hexanoic acid exhibited good linearity in the concentration range of 0.1-10 mg/L(R2=0.999 8).The limit of detection(LOD)of the method was 0.06 mg/kg,and the limit of quantification(LOQ)was 0.20 mg/kg.Three spiking levels(0.2,0.4 mg/kg,and 2.0 mg/kg)were tested in blank samples,with average recoveries ranging from 96.8% to 107.6% and relative standard deviations ranging from 0.8% to 4.1%(n=6).By using this method,16 samples of Leucosceptrum canum Smith honey and 61 samples of other honey varieties were analyzed.It was found that hexanoic acid was exclusively detected in all Leucosceptrum canum Smith honey samples,with concentrations ranging from 0.30 mg/kg to 4.14 mg/kg.Therefore,this method is easy to operate,highly sensitive,and accurate,making it suitable for determining hexanoic acid content in honey.Meanwhile,hexanoic acid can serve as a potential characteristic component of Leucosceptrum canum Smith honey for its authenticity identification and quality evaluation.
文章编号:202519021     中图分类号:    文献标志码:
基金项目:海关总署科研项目(2022HK023);云南省张进杰专家工作站(202205AF150072);海科中心自立科研课题(2023HZ03)
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