Captiva EMR-Lipid固相萃取/超高效液相色谱-串联质谱快速筛查饲料中7种真菌毒素OA北大核心CSTPCD
Captiva EMR-Lipid SPE/ultra performance liquid chromatography-tandem mass spectrometry rapid screening seven mycotoxins in feed
研究旨在采用Captiva EMR-Lipid固相萃取技术结合超高效液相色谱串联质谱法(UPLC-MS/MS)对饲料中7种真菌毒素进行快速筛查.制备后的饲料样品经84%乙腈水溶液超声(结合振摇)提取10 min,离心后经Captiva EMR-Lipid固相萃取柱一步通过式脱脂净化.然后进行UPLC-MS/MS电喷雾电离(ESI),正、负离子扫描,多反映监测模式(MRM),基质匹配外标法定量.结果表明,单个饲料样品中7种真菌毒素的提取、净化和检测分析可在30 min内完成,基质匹配标准曲线相关系数(r)均大于0.994,检出限均为2~10 μg/kg,不同水平加标浓度下的平均回收率为61.9%~123.5%,相对标准偏差(RSD)≤9.2%(n=5).研究表明,该方法前处理步骤少,易操作,筛查定性准确,检测分析通量相对较高,满足饲料中7种真菌毒素的筛查分析.
The aim of this study was to rapidly screen seven mycotoxins in feed using Captiva EMR-Lipid solid phase extraction technology combined with ultra-performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS).The prepared feed samples were extracted by ultrasonic(combined with shaking)in 84%acetonitrile aqueous solution for 10 min,centrifuged and purified by one-step pass-through degreasing on a Captiva EMR-Lipid solid-phase extraction column.Then UPLC-MS/MS Electrospray Ionization(ESI),positive and negative ion scanning,multi-reflection monitoring mode(MRM),and matrix-matched external standard quantification were carried out.The results showed that the extraction,purification and detection of seven mycotoxins in a single feed sample could be completed within 30 min,the correlation coefficient(r)of the matrix matching standard curve was greater than 0.994,the detection limit was 2~10 μg/kg,the average recovery rate was 61.9%~123.5%,and the relative standard deviation(RSD)was ≤9.2%(n=5).The study indicated that the method had few pretreatment steps,was easy to operate,the screening was qualitatively accurate,and the detection and analysis throughput was relatively high,which met the screening and analysis of seven mycotoxins in feed.
马宁;李洪波;崔海燕;张振宇
驻马店市产品质量检验检测中心,河南驻马店 463000济源职业技术学院,河南济源 459000济源市畜产品质量监测检验中心,河南济源 459000
畜牧业
超高效液相色谱-串联质谱饲料真菌毒素
ultra-performance liquid chromatography-tandem mass spectrometryfeedmycotoxins
《饲料研究》 2024 (007)
116-120 / 5
河南省济源市科技攻关项目(项目编号:19023027、20021001)
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