QuEChERS-超高效液相色譜-串聯(lián)質(zhì)譜法同時測定薏苡仁中8種真菌毒素含量

摘 要： 薏苡仁在種植、加工、運輸及貯存過程中極易受真菌毒素污染而影響下游產(chǎn)品的質(zhì)量安全，因此該實驗建立同時檢測薏苡仁中8種真菌毒素含量的方法，探究薏苡仁中真菌毒素污染情況及毒素含量，為同時檢測薏苡仁中8種真菌毒素含量提供有效方法。通過QuEChERS（Quick、Easy、Cheap、Effective、Rugged、SafeQuick easy cheap effective rugged safe）提取法作為前處理方法，使用體積分數(shù)0.1%甲酸和84%乙腈溶液為提取溶劑，以氯化鈉、無水硫酸鎂和無水硫酸鈉作為鹽析試劑，以共價有機框架材料（Covalent organic framework materials， COFs）、十八烷基硅烷鍵合硅膠（C₁₈）和N-丙基乙二胺（PSA）作為分散固相萃取凈化劑，通過多反應(yīng)監(jiān)測模式進行檢測，并以外標法進行定量。結(jié)果表明：黃曲霉毒素B₁、B₂、G₁、G₂及M₁，脫氧雪腐鐮刀菌烯醇，玉米赤霉烯酮和T-2毒素8種真菌毒素的標準曲線線性關(guān)系R²gt;0.99，3種加標濃度下回收率為62.76%～111.10%，檢出限為0.025～0.150 μg/kg，定量限為0.08～0.50 μg/kg，靈敏度高，相對標準偏差為0.38%～7.01%，穩(wěn)定性好。薏苡仁樣品中玉米赤霉烯酮和脫氧雪腐鐮刀菌烯醇檢出率較高，其他毒素檢出率低甚至無檢出，加入COFs凈化材料，可吸附截留薏苡仁樣品中復(fù)雜的油脂、糖分和色素等基質(zhì)，降低基質(zhì)干擾，滿足回收率要求。

關(guān)鍵詞：QuEChERS；真菌毒素；液質(zhì)聯(lián)用；分散固相萃取；共價有機框架材料

中圖分類號：O657.63

文獻標志碼：A

文章編號：1673-3851 （2025） 03-0254-09

引文格式：方嘉豪，潘項捷，尹峰，等. QuEChERS-超高效液相色譜-串聯(lián)質(zhì)譜法同時測定薏苡仁中8種真菌毒素含量［J］. 浙江理工大學(xué)學(xué)報（自然科學(xué)），2025，53（2）：254-262.

Reference Format： FANG Jiahao，PAN Xiangjie，YIN Feng，et al. Simultaneous determination of eight fungal toxins in coix seeds by QuEChERS ultra-high performance liquid chromatography tandem mass spectrometry［J］. Journal of Zhejiang Sci-Tech University，2025，53（2）：254-262.

Simultaneous determination of eight fungal toxins in coix seeds by QuEChERS ultra-high performance liquid chromatography tandem mass spectrometry

FANG Jiahao¹， PAN Xiangjie²， YIN Feng¹， ZHANG Shuifeng²， GAO Tong³， FENG Tinghui⁴， ZHANG Chaojun⁵， CAI Lietao⁵， LIANG Zongsuo¹， ZHANG Xiaodan¹

（1.College of Life Sciences and Medicine， Zhejiang Sci-Tech University， Hangzhou 310018， China; 2.Zhejiang Fangyuan Test Group Co.， Ltd.， Hangzhou 310018， China; 3.College of Pharmacy， Shaanxi University of Chinese Medicine， Xianyang 712046， China; 4. College of Life Sciences， Northwest Aamp;F University， Yangling 712100， China; 5. Zhejiang Kanglaite Pharmaceutical Co.， Ltd.， Hangzhou 310018， China）

Abstract：The coix seed is highly susceptible to fungal toxin contamination during cultivation， processing， transportation， and storage， which can affect the quality and safety of downstream products. Therefore， this article established a method for simultaneously detecting the content of eight fungal toxins in coix seeds， so as to explore the contamination and toxin content of fungal toxins in coix seeds， and provide an effective method for simultaneously detecting the content of eight fungal toxins in coix seeds. The QuEChERS（Quick， Easy， Cheap， Effective， Rugged and Safe） extraction method was used as a pretreatment method， with a volume concentration of 0.1% formic acid and 84% acetonitrile solution as extraction solvents， sodium chloride， anhydrous magnesium sulfate， and anhydrous sodium sulfate as salting-out reagents， covalent organic framework materials （COFs）， octadecylsilane bonded silica gel （C₁₈）， and N-propylethylenediamine （PSA） as dispersed solid-phase extraction purification agents. The detection was performed by using a multi-reaction monitoring mode and quantified by using an external standard method. The results showed that the standard curves of the eight fungal toxins， namely aflatoxin B₁， B₂， G₁， G₂， and M₁， deoxynivalenol， zearalenone， and T-2 toxin， had a linear relationship of R²gt;0.99. The recovery rates were in the range of 62.76% and 111.10% at three spiked concentrations， with a detection limit of 0.025-0.150 μg/kg and a quantification limit of 0.08-0.50 μg/kg. The sensitivity was high， and the relative standard deviation ranged from 0.38% to 7.01%， indicating good stability. The detection rates of zearalenone and deoxynivalenol in coix seed samples are relatively high， while the detection rates of other toxins are low or even non-existent. Adding COFs purification materials can adsorb and intercept complex substrates such as oil， sugar， and pigments in coix seed samples， reduce substrate interference， and meet the recovery requirements.

Key words：QuEChERS; fungal toxins; UPLC-MS; dispersed solid-phase extraction; covalent organic framework materials

0 引 言

薏苡仁是禾本科植物薏苡（Coix lacryma-jobi L.）的干燥成熟種仁^［1］，又稱薏米、苡仁等^［2］。在中國貴州、福建等多地都有種植^［3-4］。……