改良QuEChERS结合超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法测定果蔬中15种植物生长调节剂残留

莫迎; 吕敏; 张荣林; 薛亚馨; 黄燕红; 陆小康; 刘华文

doi:10.13386/j.issn1002-0306.2020.02.031

改良QuEChERS结合超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法测定果蔬中15种植物生长调节剂残留

广西-东盟食品药品安全检验检测中心, 广西南宁 530021

基金项目:

食品安全地方标准制定(修订)(桂地标食2017003号)

广西食品药品监督管理局研究项目(桂食药科2018-12)。

详细信息

作者简介:
莫迎(1970-),女,硕士,副主任药师,研究方向:食品检验与质量标准研究,E-mail:morningzai@163.com。

通讯作者:
吕敏(1986-),女,本科,主管药师,研究方向:食品检验与质量标准研究,E-mail:33785813@qq.com。

中图分类号: TS255.1
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出版历程
- 收稿日期: 2019-04-22
- 网络出版日期: 2020-11-12
- 刊出日期: 2020-01-14

Determination of 15 Plant Growth Regulators Residues in Fruits and Vegetables by Modified QuEChERS Coupled with UPLC-Q-Orbitrap HRMS

Guangxi-Asean Center Food and Drug Safety Control, Nanning 530021, China

摘要

摘要: 基于改良的QuEChERS方法,建立超高效液相色谱-四级杆/静电场轨道阱高分辨质谱法(UPLC-Q-Orbitrap HRMS)快速筛查和测定果蔬中15种植物生长调节剂残留的方法。样品以1%乙酸乙腈提取,多壁碳纳米管(MWCNTs)净化,采用Hypersil GOLD aq C₁₈色谱柱(2.1 mm×100 mm,1.9 μm)进行分离,乙腈和水(含0.1%甲酸-5 mmol/L甲酸铵)为流动相梯度洗脱,质谱采用全扫描/数据依赖的二级扫描模式,基质匹配校准曲线定量。结果显示:15种化合物在2.0~500.0 μg/L范围内,线性关系良好(r>0.990);在3个加标水平下,平均回收率为70.3%~107.2%,相对标准偏差(RSD)为1.4%~9.9%,定量限为10.0~20.0 μg/kg。该方法简单,灵敏度高,准确可靠,可对果蔬中植物生长调节剂进行快速筛查和定量分析。
- 改良QuEChERS /
- 超高效液相色谱-四级杆/静电场轨道阱高分辨质谱法 /
- 多壁碳纳米管 /
- 植物生长调节剂
Abstract: A method was developed for the simultaneous determination of 15 plant growth regulators residues in fruits and vegetables by ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry(UPLC-Q-Orbitrap HRMS)with modified QuEChERS. The samples were extracted by acetonitrile containing 1% acetic acid and purified by MWCNTs,separated on a Hypersil GOLD aq C₁₈ column(2.1 mm×100 mm,1.9 μm),gradient elution with acetonitrile and water(containing 0.1% formic acid-5 mmol/L ammonium formate). The target compounds were analyzed in full scan/data-dependent MS2(Full MS/dd-MS2)mode,and quantified by using the matrix-matched standard calibration. The results showed that the correlation coefficients was over than 0.990 in the range of 2.0~500.0 μg/mL.The three-level spiked recoveries were between from 70.3% to 107.2% with relative standard deviation from 1.4% to 9.9%. The limits of quantitation were 10.0~20.0 μg/kg. The method was simple,sensitive,accurate and suitable for the rapid screening and quantitative analysis of plant growth regulators in fruits and vegetables.
- modified QuEChERS /
- UPLC-Q-Orbitrap HRMS /
- multiwalled carbon nanotubes /
- plant growth regulators

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