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Article(id=1217781127423640346, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1217779717386715826, articleNumber=null, orderNo=null, doi=10.19812/j.cnki.jfsq11-5956/ts.20250217003, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1739721600000, receivedDateStr=2025-02-17, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1768271246057, onlineDateStr=2026-01-13, pubDate=1750780800000, pubDateStr=2025-06-25, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1768271246057, onlineIssueDateStr=2026-01-13, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1768271246057, creator=13701087609, updateTime=1768271246057, updator=13701087609, issue=Issue{id=1217779717386715826, tenantId=1146029695717560320, journalId=1149652044408987649, year='2025', volume='16', issue='12', pageStart='1', pageEnd='320', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1768270909877, creator=13701087609, updateTime=1768299620707, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1217900139386163208, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1217779717386715826, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1217900139386163209, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1217779717386715826, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=231, endPage=237, ext={EN=ArticleExt(id=1217781127851459381, articleId=1217781127423640346, tenantId=1146029695717560320, journalId=1149652044408987649, language=EN, title=Determination of 17-pentatriacontene in honey by gas chromatography-flame ionization detection and gas chromatography-mass spectrometry, columnId=1151895321388347923, journalTitle=Journal of Food Safety & Quality, columnName=Food Analysis and Detection, runingTitle=null, highlight=null, articleAbstract=

Objective To establish 2 kinds of methods for the determination of 17-pentatriacontene in honey by gas chromatography-flame ionization detection (GC-FID) and gas chromatography-mass spectrometry (GC-MS). Methods After dissolved in water, the sample was extracted with petroleum ether, purified on a florisil cartridge, separated by DB-5MS column (15 m×0.25 mm, 0.25 μm), and determined by GC-FID and GC-MS, then quantified by external standard method. Results The GC-FID and GC-MS were quantified using matrix-free standard curve and matrix-matched standard curve respectively, with limits of quantification of 1.0 mg/kg and 0.5 mg/kg, linear ranges of 1-100 mg/kg and 0.5-40.0 mg/kg, and recovery rates ranging from 88.9% to 94.5% and from 91.2% to 98.2%, respectively. The relative standard deviations were 4.0%-6.4% and 4.6%-7.3%, respectively. The results of the 2 kinds of methods were basically consistent, with a relative deviation of no more than 2.4%. The proposed methods were applied to 158 honey samples of Apis cerana honey and Apis mellifera honey, 17-pentatriacontene was only detected in Apis cerana honey, with a content range of 0.58-51.10 mg/kg. Conclusion The accuracy and precision of the GC-FID and GC-MS methods established in this study are both good, and the 2 kinds of methods can be applied to the determination of 17-pentatriacontene in honey. The results of real sample tested indicate that 17-pentatriacontene can be used as a characteristic marker for Apis cerana honey.

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目的 建立气相色谱-火焰离子化检测法(gas chromatography-flame ionization detection, GC-FID)和气相色谱-质谱法(gas chromatography-mass spectrometry, GC-MS)测定蜂蜜中17-三十五烯含量的方法。方法 样品经水溶解, 石油醚提取, 弗罗里硅土柱固相萃取净化, DB-5MS色谱柱(15 m×0.25 mm, 0.25 μm)分离, 分别采用GC-FID和GC-MS进行测定, 外标法定量。结果 GC-FID和GC-MS分别采用溶剂标准曲线和基质匹配标准曲线定量, 定量限分别为1.0 mg/kg和0.5 mg/kg, 线性范围分别为1~100 mg/kg和0.5~40.0 mg/kg, 添加回收率范围分别为88.9%~94.5%和91.2%~98.2%, 相对标准偏差范围分别为4.0%~6.4%和4.6%~7.3%; 两种方法检测结果基本一致, 相对偏差不超过2.4%。使用所建方法检测158批次中华蜜蜂蜂蜜和意大利蜜蜂蜂蜜, 结果仅在中华蜜蜂蜂蜜中检出17-三十五烯, 其含量范围为0.58~51.10 mg/kg。结论 本研究建立的GC-FID和GC-MS具有较高的灵敏度和准确度, 适用于蜂蜜中17-三十五烯的测定; 样品检测结果确证了17-三十五烯可以作为中华蜜蜂蜂蜜的特征标识物。

, correspAuthors=崔宗岩, authorNote=null, correspAuthorsNote=
*崔宗岩(1983—), 男, 博士, 正高级工程师, 主要研究方向为蜂蜜真伪鉴别与质量安全检测。E-mail:
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温昊松(1989—), 男, 工程师, 主要研究方向为食品质量安全检测。E-mail:

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温昊松(1989—), 男, 工程师, 主要研究方向为食品质量安全检测。E-mail:

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温昊松(1989—), 男, 工程师, 主要研究方向为食品质量安全检测。E-mail:

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注: 图中不同小写字母表示存在显著差异(P<0.05)。

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LODs, LOQs, linear range, linear equations and linear correlation coefficients of 17-pentatriacontene

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检测方法 LODs/(mg/kg) LOQs/(mg/kg) 线性范围/(mg/kg) 线性回归方程 相关系数(r2)
GC-FID 0.30 1.0 1~100 Y=0.77X+0.261 0.9998
GC-MS 0.15 0.5 0.5~40.0 Y=723X-1220.9 0.9991
), ArticleFig(id=1217833927696368377, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217781127423640346, language=CN, label=表1, caption=

17-三十五烯的LODs、LOQs、线性范围、线性方程和相关系数

, figureFileSmall=null, figureFileBig=null, tableContent=
检测方法 LODs/(mg/kg) LOQs/(mg/kg) 线性范围/(mg/kg) 线性回归方程 相关系数(r2)
GC-FID 0.30 1.0 1~100 Y=0.77X+0.261 0.9998
GC-MS 0.15 0.5 0.5~40.0 Y=723X-1220.9 0.9991
), ArticleFig(id=1217833927830586118, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217781127423640346, language=EN, label=Table 2, caption=

Experimental results of labeling recoveries of 17-pentatriacontene (n=6)

, figureFileSmall=null, figureFileBig=null, tableContent=
检测方法 添加水平/(mg/kg) 平均回收率/% RSDs
/%
GC-FID 1.0 88.9 6.4
2.0 94.2 5.1
10.0 94.5 4.0
GC-MS 0.5 91.2 7.3
2.5 92.7 7.0
5.0 98.2 4.6
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17-三十五烯的加标回收率实验结果(n=6)

, figureFileSmall=null, figureFileBig=null, tableContent=
检测方法 添加水平/(mg/kg) 平均回收率/% RSDs
/%
GC-FID 1.0 88.9 6.4
2.0 94.2 5.1
10.0 94.5 4.0
GC-MS 0.5 91.2 7.3
2.5 92.7 7.0
5.0 98.2 4.6
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气相色谱-火焰离子化检测法和气相色谱-质谱法检测蜂蜜中17-三十五烯含量
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温昊松 , 黄学者 , 张悦 , 刘晓茂 , 贾光群 , 崔宗岩 *
食品安全质量检测学报 | 食品分析与检测 2025,16(12): 231-237
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食品安全质量检测学报 | 食品分析与检测 2025, 16(12): 231-237
气相色谱-火焰离子化检测法和气相色谱-质谱法检测蜂蜜中17-三十五烯含量
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温昊松 , 黄学者, 张悦, 刘晓茂, 贾光群, 崔宗岩*
作者信息
  • 秦皇岛海关技术中心, 秦皇岛 066004

    • 温昊松(1989—), 男, 工程师, 主要研究方向为食品质量安全检测。E-mail:

通讯作者:

*崔宗岩(1983—), 男, 博士, 正高级工程师, 主要研究方向为蜂蜜真伪鉴别与质量安全检测。E-mail:
Determination of 17-pentatriacontene in honey by gas chromatography-flame ionization detection and gas chromatography-mass spectrometry
Hao-Song WEN , Xue-Zhe HUANG, Yue ZHANG, Xiao-Mao LIU, Guang-Qun JIA, Zong-Yan CUI*
Affiliations
  • Technology Center of Qinhuangdao Customs, Qinhuangdao 066004, China
出版时间: 2025-06-25 doi: 10.19812/j.cnki.jfsq11-5956/ts.20250217003
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目的 建立气相色谱-火焰离子化检测法(gas chromatography-flame ionization detection, GC-FID)和气相色谱-质谱法(gas chromatography-mass spectrometry, GC-MS)测定蜂蜜中17-三十五烯含量的方法。方法 样品经水溶解, 石油醚提取, 弗罗里硅土柱固相萃取净化, DB-5MS色谱柱(15 m×0.25 mm, 0.25 μm)分离, 分别采用GC-FID和GC-MS进行测定, 外标法定量。结果 GC-FID和GC-MS分别采用溶剂标准曲线和基质匹配标准曲线定量, 定量限分别为1.0 mg/kg和0.5 mg/kg, 线性范围分别为1~100 mg/kg和0.5~40.0 mg/kg, 添加回收率范围分别为88.9%~94.5%和91.2%~98.2%, 相对标准偏差范围分别为4.0%~6.4%和4.6%~7.3%; 两种方法检测结果基本一致, 相对偏差不超过2.4%。使用所建方法检测158批次中华蜜蜂蜂蜜和意大利蜜蜂蜂蜜, 结果仅在中华蜜蜂蜂蜜中检出17-三十五烯, 其含量范围为0.58~51.10 mg/kg。结论 本研究建立的GC-FID和GC-MS具有较高的灵敏度和准确度, 适用于蜂蜜中17-三十五烯的测定; 样品检测结果确证了17-三十五烯可以作为中华蜜蜂蜂蜜的特征标识物。

17-三十五烯  /  中华蜜蜂蜂蜜  /  意大利蜜蜂蜂蜜  /  特征成分  /  气相色谱-火焰离子化检测法  /  气相色谱-质谱法

Objective To establish 2 kinds of methods for the determination of 17-pentatriacontene in honey by gas chromatography-flame ionization detection (GC-FID) and gas chromatography-mass spectrometry (GC-MS). Methods After dissolved in water, the sample was extracted with petroleum ether, purified on a florisil cartridge, separated by DB-5MS column (15 m×0.25 mm, 0.25 μm), and determined by GC-FID and GC-MS, then quantified by external standard method. Results The GC-FID and GC-MS were quantified using matrix-free standard curve and matrix-matched standard curve respectively, with limits of quantification of 1.0 mg/kg and 0.5 mg/kg, linear ranges of 1-100 mg/kg and 0.5-40.0 mg/kg, and recovery rates ranging from 88.9% to 94.5% and from 91.2% to 98.2%, respectively. The relative standard deviations were 4.0%-6.4% and 4.6%-7.3%, respectively. The results of the 2 kinds of methods were basically consistent, with a relative deviation of no more than 2.4%. The proposed methods were applied to 158 honey samples of Apis cerana honey and Apis mellifera honey, 17-pentatriacontene was only detected in Apis cerana honey, with a content range of 0.58-51.10 mg/kg. Conclusion The accuracy and precision of the GC-FID and GC-MS methods established in this study are both good, and the 2 kinds of methods can be applied to the determination of 17-pentatriacontene in honey. The results of real sample tested indicate that 17-pentatriacontene can be used as a characteristic marker for Apis cerana honey.

17-pentatriacontene  /  Apis cerana honey  /  Apis mellifera honey  /  characteristic compounds  /  gas chromatography-flame ionization detection  /  gas chromatography-mass spectrometry
温昊松, 黄学者, 张悦, 刘晓茂, 贾光群, 崔宗岩. 气相色谱-火焰离子化检测法和气相色谱-质谱法检测蜂蜜中17-三十五烯含量. 食品安全质量检测学报, 2025 , 16 (12) : 231 -237 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20250217003
Hao-Song WEN, Xue-Zhe HUANG, Yue ZHANG, Xiao-Mao LIU, Guang-Qun JIA, Zong-Yan CUI. Determination of 17-pentatriacontene in honey by gas chromatography-flame ionization detection and gas chromatography-mass spectrometry[J]. Journal of Food Safety & Quality, 2025 , 16 (12) : 231 -237 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20250217003
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0 引言
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我国蜜蜂主要由中华蜜蜂(Apis cerana, 简称中蜂)和意大利蜜蜂(Apis mellifera, 简称意蜂)两大种群组成[1]。意蜂具有繁殖力强、产蜜量大的优势, 现为我国饲养的主要蜂种。而作为本土蜂种的中蜂则个体小, 繁育慢, 蜂蜜生产周期长且产量远低于意蜂。中蜂嗅觉敏感, 善于发现和采集分散花源, 酿造的百花蜜也称“土蜂蜜”, 具有清热解毒、补中润燥、养颜、抗衰老等功效, 近年来深受本土消费者的信赖与追捧。中蜂蜂蜜市场价格高昂, 为普通意蜂蜂蜜的3~5倍以上[2], 因此存在用意蜂蜂蜜冒充或掺入中蜂蜂蜜的造假现象。
目前用于鉴别中蜂蜂蜜和意蜂蜂蜜的方法主要基于: 理化性质差异性[3-5]、挥发性成分及含量差异[6-8]、王浆主蛋白成分含量差异[9-11]、基因检测技术[12-15]、代谢组学技术[16-17]、特征成分含量差异[18-23]等方面。近年研究多通过对蜂蜜化学特征的一致或异常信号进行检测分析, 实现对蜂蜜的真实性鉴别。现有研究表明, 17-三十五烯为中蜂蜂蜜中特有的烃类成分, 来源于中蜂蜂蜡[24], 该化合物能够在蜂蜜基质中稳定存在, 且提取、测定简便。检测烃类物质最常用的仪器方法有气相色谱-火焰离子化检测法(gas chromatography-flame ionization detection, GC-FID)[25-27]和气相色谱-质谱法(gas chromatography-mass spectrometry, GC-MS)[28-29]。本研究团队已参与制定了GB/T 43448—2023《蜂蜜中17-三十五烯含量的测定 气相色谱质谱法》, 该方法具有选择性强, 定性准确, 灵敏度和准确度高等优点, 但仪器成本较高。本研究进一步优化了样品仪器条件和前处理条件, 建立了蜂蜜中17-三十五烯检测的GC-FID并与GC-MS进行了比对, 并采用建立的方法对158批次中蜂和意蜂蜂蜜中17-三十五烯进行了检测和分析, 为中蜂蜂蜜的特异性鉴别提供技术支撑和数据支撑。
1 材料与方法
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1.1 仪器、试剂与样品
7890B-5977B型气相色谱-质谱仪(配有电子轰击源)(electron impact, EI)、6890N型气相色谱仪(配有FID)、DB-5MS型毛细管柱(5%苯基-甲基聚硅氧烷, 15 m×0.25 mm, 0.25 μm)(美国安捷伦公司); SGH-300型高纯氢气发生器(北京东方精华苑科技有限公司); BL-320S型分析天平(感量0.001 g, 日本岛津公司); XS205型分析天平(感量0.1 mg, 瑞士Mettler Toledo公司); X3R型高速离心机(美国Thermo Fisher Scientific公司); 佛罗里硅土(Florisil)固相萃取柱(1 g/6 mL, 北京迪马科技公司); 微孔滤膜(0.22 μm, 江苏绿盟科学仪器有限公司)。
异辛烷、正己烷、石油醚(沸程35~60 ℃)(色谱纯, 北京迪马科技公司); 17-三十五烯[CAS号: 6971-40-0, 纯度≥98%, 阿拉丁试剂(上海)有限公司]; 高纯氦气(纯度≥99.999%, 辽宁营口嘉禾气体有限公司)。
意蜂蜂蜜(包括洋槐蜜、油菜蜜、椴树蜜等)和中蜂蜂蜜样品共158批, 均于2022—2023年间直接购自蜂农, 为纯天然蜂蜜。
1.2 标准溶液配制
标准储备液: 称取适量17-三十五烯标准物质, 用异辛烷溶解并定容, 配制成质量浓度为1 mg/mL的标准储备液。
1.3 方法
1.3.1 样品的提取
称取试样5 g(精确至0.01 g)置于50 mL离心管, 加入水10 mL, 涡旋混匀。加入石油醚20 mL, 振荡30 min, 10000 r/min离心10 min, 收集上清液。残渣中加入石油醚20 mL, 重复提取1次, 合并2次提取液, 40 ℃水浴氮气吹干, 用正己烷2 mL复溶, 涡旋混匀, 获得提取液待净化。
1.3.2 样品的净化
将Florisil固相萃取柱用正己烷6 mL活化后, 取提取液上样至固相萃取柱, 用正己烷10 mL洗脱, 收集所有流出物, 40 ℃水浴氮气吹干, 加入正己烷1 mL, 涡旋1 min溶解残余物, 过滤至进样瓶, 供GC-FID和GC-MS测定。
1.4 仪器条件
GC条件: 进样口温度: 300 ℃; 进样模式: 分流进样, 分流比: 10:1; 载气: 高纯氦气(纯度≥99.999%), 流速: 1.5 mL/min; 色谱柱: DB-5MS毛细管柱(15 m×0.25 mm, 0.25 μm); 色谱柱升温程序: 起始温度为60 ℃, 保持1 min, 然后以30 ℃/min升至300 ℃, 保持5 min。
FID条件: FID检测器温度: 300 ℃; 氢气流量: 40 mL/min; 空气流量: 450 mL/min; 尾吹气(高纯氮气)流量: 30 mL/min。
MS条件: 离子源温度: 230 ℃; 传输线温度: 300 ℃; 检测方式: 选择离子扫描(selected ion monitoring, SIM)。
1.5 基质效应评价方法
由于共提取物的存在, 样品溶液注入仪器后, 分析目标物的信号可能会增强或者减弱, 进而产生基质效应(matrix effect, ME), 本研究通过比较基质匹配标准曲线的斜率与溶剂标准曲线的斜率来评价ME, 按照公式(1)计算。

ME/%=[基质匹配标准曲线的斜率/溶剂标准曲线的斜率]×100%

1.6 数据处理
使用美国安捷伦公司GC化学工作站, MassHunter QuantAnalysis软件和OriginPro 2018C软件进行相关数据处理、分析和作图。
2 结果与分析
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2.1 色谱条件的选择
根据17-三十五烯弱极性的特点, 以及相似相溶的色谱分配原理, 选择弱极性色谱柱进行分析; 由于该化合物的质量数比较大, 故选择短柱, 经验证, 在15 m的DB-5MS色谱柱(15 m×0.25 mm, 0.25μm)上, 目标物有较好的保留及分离效果。
2.2 质谱条件的优化
将17-三十五烯标准溶液注入GC-MS, 在m/z 40~550范围内进行全扫描, 确定目标物的保留时间为10.0 min, 获得其全扫描质谱图见图1A; 进而选择强度较高的离子(97.1、111.1、125.1、490.6)作为目标物特征离子, 建立SIM方法, 进样获得其SIM谱图见图1B。其中质量数较小的3个离子容易受背景干扰, 而选择490.6进行定量, 尽管其绝对响应低于其他离子, 但由于该离子背景噪音远低于其他离子, 使得其信噪比(S/N)更高, 也就是获得了更高的方法灵敏度, 因而选择490.6作为定量离子。标准溶液(质量浓度为200 μg/mL)的GC-MS色谱图和GC色谱图见图2。
2.3 提取条件的优化
烃类物质的提取一般选用液液萃取法, 常用振荡提取方式, 本研究选取代表性中蜂蜂蜜, 对提取试剂、萃取时间、萃取次数分别进行了优化(n=3)。
(1)提取溶剂
烃类物质易溶于石油醚、二氯甲烷、正己烷等有机试剂[30], 考察了石油醚(沸程35~60 ℃)、石油醚(沸程60~90 ℃)、二氯甲烷、正己烷、正己烷:二氯甲烷(1:1, V:V) 5种试剂的提取效率。结果(图3A)表明, 石油醚(沸程35~60 ℃)的提取效率显著高于其他试剂, 因而选择35~60 ℃沸程的石油醚作为提取溶剂。
(2)萃取时间
以石油醚(沸程35~60 ℃)作为提取试剂, 对比了萃取时间分别为5、15、30、45、60、90 min的提取效率, 结果(图3B)表明, 萃取时间在5~30 min内随时间增加萃取效率逐渐提高, 超过30 min萃取效率无显著变化, 表明萃取30 min能够使得目标物充分提取, 因而选择萃取时间为30 min。
(3)萃取次数
以石油醚(沸程35~60 ℃)作为提取试剂, 振荡30 min条件进行提取次数的研究, 分别收集第1~4次提取液进行测定, 结果表明, 前2次提取率达98%以上。
综上, 本研究选择石油醚(沸程35~60 ℃)作为提取试剂, 振荡30 min, 提取2次。
2.4 净化条件的选择
蜂蜜样品含有糖、蛋白质、色素、有机酸、脂肪酸等组分, 会对目标物的定性定量产生一定影响。特别是中蜂蜂蜜, 提取液浓缩后颜色较深, 直接进样会影响目标物的定量且会对色谱系统产生污染。本研究选用固相萃取法进行净化, 经实验表明Florisil柱净化效果比较显著, 可以去除样品中色素等干扰物质, 且不影响目标物的回收率。
2.5 基质效应评价
采用1.5所述ME评价方法, 一般ME值在0.8~1.2之间, 认为其ME可以忽略, ME>1.2认为存在基质增强效应, ME<0.8则存在基质抑制效应。本研究计算得到GC-FID和GC-MS的ME值分别为1.01和1.35, 表明前者没有ME, 而后者存在基质增强效应, 故二者分别选用溶剂标准曲线和基质匹配标准曲线进行定量。
2.6 方法学评价
2.6.1 线性范围、相关系数及定量限
将质量浓度为5、10、20、50、200、500 μg/mL的系列溶剂标准工作溶液和2.5、5.0、10.0、20.0、50.0、100.0、200.0 μg/mL的系列基质匹配标准工作溶液, 分别采用GC-FID和GC-MS进行测定, 并绘制标准曲线, 得出线性方程。以不低于3倍信噪比对应的样品浓度为方法检出限(limit of detection, LOD), 不低于10倍信噪比对应的样品浓度为方法定量限(limit of quantitation, LOQ)。2种方法的LOD和LOQ、线性范围、线性方程、线性相关系数(r2)见表1。结果表明, GC-FID和GC-MS的线性相关系数(r2)均高于0.9990, 线性关系均良好。两种方法对比, GC-MS的LOD和LOQ更低, 为GC-FID法的1/2, 其灵敏度更高, 因为GC-MS法选择性更强, 选择离子背景噪音较低, 可以获得更高的信噪比; 而GC-FID法虽然灵敏度略低, 但其线性范围更宽, 且线性关系更好一些。
2.6.2 方法准确度和精密度
利用本研究建立的检测方法, 进行空白样品中低、中、高3个浓度水平(LOQ、2LOQ、10LOQ)的加标回收实验(n=6), GC-FID和GC-MS平均回收率分别在88.9%~94.5%、91.2%~98.2%之间, 相对标准偏差(relative standard deviations, RSDs)分别在4.0%~6.4%、4.6%~7.3%之间, 表明方法准确度和精密度均较高, 空白样品及各水平添加色谱图见图4, 具体结果见表2。
2.7 实际样品的检测
由于GC-MS相对于GC-FID具有更高的灵敏度, 采用GC-MS对采集的78批次中蜂蜂蜜(均为百花蜜)和80批次意蜂蜂蜜(包括洋槐蜜、荆条蜜、油菜蜜、枣花蜜、椴树蜜、荔枝蜜、百花蜜等)中的17-三十五烯含量进行检测。检测结果表明: 80批次意蜂蜂蜜均未检出, 而78批次中蜂蜂蜜样品均有不同浓度检出, 检出率为100%, 其含量范围为0.58~51.10 mg/kg, 说明17-三十五烯是中蜂蜂蜜的特征标识物。分布情况见图5A, 从小提琴图中数据密度分布可知, 中蜂蜂蜜样品的17-三十五烯集中分布在5.30~9.90 mg/kg之间, 含量中位数为: 7.35 mg/kg, 整体上中蜂蜂蜜中的17-三十五烯含量分布比较集中。
对GC-FID和GC-MS的定量结果进行比对, 随机在上述样品中选择15个含量不同的中蜂蜂蜜样品采用GC进行定量, 结果(图5B)表明: 2种方法的检测结果基本吻合, 相对偏差不超过2.4%。GC-FID具有稳定性好、仪器成本低的优点, GC-MS则具有灵敏度高、选择性好的优点。
3 结论
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本研究建立了GC-FID和GC-MS检测蜂蜜中的17-三十五烯含量的方法。在优化的实验条件下, 两个方法均具有高灵敏和高准确度, GC-FID和GC-MS的定量限分别为1.0 mg/kg和0.5 mg/kg, 且实际样品检测结果基本一致, 均适用于蜂蜜中17-三十五烯的测定。对78批中蜂蜂蜜和80批意蜂蜂蜜样品检测结果表明, 17-三十五烯仅在中蜂蜂蜜中检出, 且检出率为100%, 表明该化合物可以作为中蜂蜂蜜的特征标志物。本研究所建立的检测方法和检测结果可为中蜂蜂蜜的鉴别和品质评价提供技术和数据支撑。
基金
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  • 海关总署科研项目(2022HK023)
文献
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2025年第16卷第12期
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doi: 10.19812/j.cnki.jfsq11-5956/ts.20250217003
  • 接收时间：2025-02-17
  • 首发时间：2026-01-13
  • 出版时间：2025-06-25
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  • 收稿日期：2025-02-17
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海关总署科研项目(2022HK023)
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    秦皇岛海关技术中心, 秦皇岛 066004

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*崔宗岩(1983—), 男, 博士, 正高级工程师, 主要研究方向为蜂蜜真伪鉴别与质量安全检测。E-mail:
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2种不同金属材料的力学参数
科
Family		 属数
Number of
genus		 种数
Number of
species		 占总种数比例
Percentage of
total species (%)		 属
Genus		 种数
Number of
species		 占总种数比例
Percentage of total
species (%)
鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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