GC-MS/MS法测定茶鲜叶中20种邻苯二甲酸酯类化合物

茶叶科学 ›› 2025, Vol. 45 ›› Issue (4): 625-636.

GC-MS/MS法测定茶鲜叶中20种邻苯二甲酸酯类化合物

孙渝^1,2, 周利², 张新富^1,*, 孙荷芝^2,*

1.青岛农业大学园艺学院,山东青岛 266109;
2.中国农业科学院茶叶研究所农产品质量安全研究中心,浙江杭州 310008

收稿日期:2024-12-24 修回日期:2025-01-20 出版日期:2025-08-15 发布日期:2025-08-15
通讯作者: *zxftea@163.com;sunhezhi@tricaas.com
作者简介:孙渝,女,硕士研究生,主要从事污染物检测方面的研究。
基金资助:
“十四五”国家重点研发计划重点专项（2022YFD1600803）、中国农业科学院创新工程项目（CAAS ASTIP-TRICAAS）、崂山茶产业创新团队项目（SDGP370212000202402000729）

Determination of 20 Phthalate Acid Esters in Tea Leaves by GC-MS/MS

SUN Yu^1,2, ZHOU Li², ZHANG Xinfu^1,*, SUN Hezhi^2,*

1. College of Plant Protection, Qingdao Agricultural University, Qingdao 266109, China;
2. Research Center of Quality Safety for Agricultural Products, Tea Research Institute, Chinese Academy of Agricultural Sciences, Hangzhou 310008, China

Received:2024-12-24 Revised:2025-01-20 Online:2025-08-15 Published:2025-08-15

摘要/Abstract

摘要： 建立了气相色谱-串联质谱（Gas chromatography-tandem mass spectrometry,GC-MS/MS）同时测定茶鲜叶中20种邻苯二甲酸酯类化合物的分析方法。茶鲜叶中的邻苯二甲酸酯类化合物经0.1%乙酸乙腈提取、氯化钠盐析、Florisil固相萃取柱净化、乙腈定容,色谱程序升温分离,多反应监测模式扫描（Multiple reaction monitoring,MRM）,外标法定量。通过优化样品提取、净化以及色谱条件,目标化合物在0.010~2.0 mg·kg^-1范围内线性良好,决定系数（R²）>0.995 5;在0.010、0.10 mg·kg^-1和1.0 mg·kg^-1 3个添加水平下,平均回收率在70%~118%,相对标准偏差（RSD）<17.8%;方法的定量限为0.010~0.10 mg·kg^-1。该方法稳定、可靠,可满足茶树鲜叶中邻苯二甲酸酯类化合物的检测需要。

关键词: 茶鲜叶, 气相色谱-串联质谱, 邻苯二甲酸酯类化合物

Abstract: In this paper, an analytical method for the simultaneous determination of 20 phthalate esters in tea fresh leaves was developed by gas chromatography-tandem mass spectrometry (GC-MS/MS). The phthalate esters in tea fresh leaves were extracted by 0.1% acetonitrile acetate, salted out with sodium chloride, cleaned up with a florisil solid phase extraction column, resolved with acetonitrile, separated by temperature programmed chromatography, monitored with multiple reaction monitoring (MRM) mode, and quantified by the external standard method. Through the optimization of sample extraction, purification and chromatographic conditions, good linearity of the target compounds was obtained in the concentration range of 0.010-2.0 mg·kg^-1 with the corresponding coefficient of determination R²>0.995 5. The average recoveries ranged from 70% to 118% at the three spiked levels of 0.010 mg·kg^-1, 0.10 mg·kg^-1 and 1.0 mg·kg^-1, with the relative standard deviations (RSDs) of <17.8%. The limits of quantification were 0.010~0.050 mg·kg^-1. The method is stable and reliable, and it can meet the needs of the determination of phthalate acid esters in tea fresh leaves.

Key words: tea fresh leaves, gas chromatography-tandem mass spectrometry, phthalate acid esters

中图分类号:

孙渝, 周利, 张新富, 孙荷芝. GC-MS/MS法测定茶鲜叶中20种邻苯二甲酸酯类化合物[J]. 茶叶科学, 2025, 45(4): 625-636.

SUN Yu, ZHOU Li, ZHANG Xinfu, SUN Hezhi. Determination of 20 Phthalate Acid Esters in Tea Leaves by GC-MS/MS[J]. Journal of Tea Science, 2025, 45(4): 625-636.

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