[1]张丽,刘腾飞,陆皓茜,等.茶鲜叶中多环芳烃液相色谱检测方法的构建及应用[J].江苏农业学报,2026,42(04):826-834.[doi:doi:10.3969/j.issn.1000-4440.2026.04.019]
　ZHANG Li,LIU Tengfei,LU Haoqian,et al.Establishment and application of a liquid chromatography method for detection of polycyclic aromatic hydrocarbons in fresh tea leaves[J].,2026,42(04):826-834.[doi:doi:10.3969/j.issn.1000-4440.2026.04.019]
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茶鲜叶中多环芳烃液相色谱检测方法的构建及应用()

江苏农业学报[ISSN:1006-6977/CN:61-1281/TN]

卷:
42
期数:
2026年04期
页码:
826-834
栏目:
加工贮藏·质量安全
出版日期:
2026-04-30

文章信息/Info

Title:
Establishment and application of a liquid chromatography method for detection of polycyclic aromatic hydrocarbons in fresh tea leaves
作者:
张丽1; 刘腾飞2; 3; 陆皓茜2; 陆丽华4; 杨代凤2; 朱莹莹1; 李德佳1
(1.苏州职业技术大学药食同源大健康创新联合体,江苏苏州215104；2.江苏太湖地区农业科学研究所,江苏苏州215106；3.南京农业大学食品科学技术学院,江苏南京210095；4.苏州市吴中区金庭镇农林服务站,江苏苏州215156)
Author(s):
ZHANG Li1; LIU Tengfei2; 3; LU Haoqian2; LU Lihua4; YANG Daifeng2; ZHU Yingying1; LI Dejia1
(1.Food & Medicine Homology Big Health Innovation Consortium, Suzhou Polytechnic University, Suzhou 215104, China;2.Jiangsu Taihu Area Institute of Agricultural Sciences, Suzhou 215106, China;3.College of Food Science and Technology, Nanjing Agricultural University, Nanjing 210095, China;4.Suzhou Wuzhong Jinting Town Agriculture and Forestry Service Station, Suzhou 215156, China)
关键词:
碧螺春; 茶鲜叶; 多环芳烃; 高效液相色谱
Keywords:
Biluochun; fresh tea leaves; polycyclic aromatic hydrocarbons; high-performance liquid chromatography
分类号:
S571.101
DOI:
doi:10.3969/j.issn.1000-4440.2026.04.019
文献标志码:
A
摘要:
为了观察茶鲜叶中的多环芳烃(PAH)变化,用超声提取-固相萃取法对PAH进行分离净化,并对比不同提取、净化条件下的PAH回收率,得到最佳前处理方案,建立基于高效液相色谱(HPLC)的茶鲜叶中PAH的检测方法。结果显示,茶鲜叶中PAH的最优前处理、液相色谱检测条件如下:取3.0 g样品,以15 mL丙酮-正己烷(体积比1∶1)作为提取剂进行超声提取,首先将提取液过弗罗里硅土、N-丙基乙二胺双填料固相萃取柱进行净化,然后用10 mL正己烷-二氯甲烷(体积比3∶7)进行淋洗,再用Aglient ZORBAX Eclipse PAH色谱柱(4.6 mm×250.0 mm, 5 μm)进行分离。以乙腈-水为流动相进行梯度洗脱,流速为2.0 mL/min,用HPLC-荧光检测器检测,用溶剂外标法进行定量分析。结果表明,15种PAH在0.005～0.500 mg/L质量浓度范围内的线性关系良好,相关系数(r)均不低于0.999 9,平均回收率为72.6%～115.1%,相对标准偏差(n=6)为1.0%～16.5%,检出限为0.000 2～0.003 0 mg/kg,定量限均为0.005 mg/kg。将本研究方法应用于碧螺春茶鲜叶中PAH的测定分析,研究结果显示,样品中PAH的含量为6.55～122.67 μg/kg,平均含量为56.75 μg/kg,并以3环、4环PAH为主,其中芴的检出率(96%)、平均含量(27.82 μg/kg)均最高。由研究结果看出,本研究方法的准确度、精密度和灵敏度良好,可为开展茶鲜叶中PAH的相关研究提供重要技术支持。
Abstract:
To monitor changes of polycyclic aromatic hydrocarbons (PAHs) in fresh tea leaves, PAHs were separated and purified by ultrasonic extraction-solid phase extraction (UE-SPE). By comparing the recovery rates of PAHs under different extraction and purification conditions, the optimal pretreatment protocol was obtained, and a method for the determination of PAHs in fresh tea leaves based on high performance liquid chromatography (HPLC) was established. The optimal pretreatment and liquid chromatography detection conditions for PAHs in fresh tea leaves were determined as follows: 3.0 g of sample was extracted ultrasonically with 15 mL of acetone-n-hexane (1 to 1, v/v) as the extraction solvent. The extract was first purified through a dual-sorbent SPE column packed with Florisil and N-propylethylenediamine (PSA), then eluted with 10 mL of n-hexane-dichloromethane (3 to 7, v/v). Separation was performed on an Agilent ZORBAX Eclipse PAH column (4.6 mm×250 mm, 5 μm) using gradient elution with acetonitrile-water as the mobile phase at a flow rate of 2.0 mL/min. Detection was carried out by HPLC with a fluorescence detector (HPLC-FLD), and quantification was performed using the external standard method. The results showed that good linearity was observed for the 15 PAHs in the concentration range of 0.005-0.500 mg/L, with correlation coefficients (r) greater than 0.999 9. The average spiked recoveries ranged from 72.6% to 115.1%, with relative standard deviations (RSDs, n=6) of 1.0%-16.5%. The limits of detection (LODs) were 0.000 2-0.003 0 mg/kg, and the limit of quantitation (LOQ) was 0.005 mg/kg. The developed method was applied to the determination of PAHs in fresh Biluochun tea leaves. The results showed that the total PAH concentrations ranged from 6.55 μg/kg to 122.67 μg/kg, with a mean concentration of 56.75 μg/kg. The PAH profile was dominated by 3- and 4-ring PAHs, among which fluorene exhibited the highest detection frequency (96%) and mean concentration (27.82 μg/kg). These results indicate that the developed method exhibits satisfactory accuracy, precision, and sensitivity, providing important technical support for PAH-related research in fresh tea leaves.

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备注/Memo

备注/Memo:
收稿日期：2025-06-10基金项目：江苏高校“青蓝工程”优秀青年骨干教师培养项目(2024)；江苏省职业院校学生创新创业培育计划项目(GX-2024-0660)；国家重点研发计划项目(2024YFF1105705)；苏州职业技术大学药食同源大健康创新联合体项目(KY2025PT09)作者简介：张丽(1986-),女,山西灵石人,博士,副教授,主要从事农产品质量安全研究。(E-mail)zhangli_szd@163.com通讯作者：刘腾飞,(E-mail)liutengfei@jaas.ac.c
更新日期/Last Update: 2026-05-11