摘要
本研究旨在建立同时测定玉米中4种链格孢霉毒素——交链孢酚(AOH)、交链胞酚单甲醚(AME)、细交链孢菌酮酸(TeA)及腾毒素(TEN)的QuEChERS-超高效液相色谱-串联质谱(UHPLC-MS/MS)法,并利用该方法检测山东省30份饲用玉米AOH、AME、TeA和TEN污染的背景值。将玉米样品加水溶解,用0.1%甲酸-乙腈溶液提取,氯化钠盐析,安捷伦EC-C18柱(100 mm×2.1 mm,2.7μm)为试验色谱柱,分别用乙腈(流动相A)和超纯水(流动相B)梯度洗脱,负离子电离模式(ESI-)作为电离条件,多反应离子监测模式(MRM)定量与定性分析,通过标准曲线、准确度和精密度试验评价建立的QuEChERS-UHPLC-MS/MS法。结果表明:4种链格孢霉毒素在1~100μg/L时线性关系良好;在5、10和50μg/kg 3种加标情况下,TeA、AOH、AME和TEN的加标回收率分别为74.70%~84.60%、 77.94%~103.84%、 72.61%~102.14%和71.16%~73.16%,相对标准偏差(RSD)分别为4.08%~8.36%、2.03%~4.07%、1.80%~4.61%和1.99%~2.40%。使用该方法检测的山东省30份饲用玉米中,TEN未检出,AOH、AME、TeA的检出率分别为96.67%、93.30%、40.00%。综上可知,本试验所建立的QuEChERS-UHPLC-MS/MS法,准确度、精密度高和稳定性好,可作为玉米中AOH、AME、TeA和TEN的检测方法;山东省饲用玉米样品中AOH、AME和TeA的检出率较高,应当引起重视。
The purpose of this study was to establish an QuEChERS-ultra-high performance liquid chromatography tandem mass spectrometry(QuEChERS-UHPLC-MS/MS)method for the simultaneous detection of four Alternaria toxins—alternaria(AOH),alternariol monomethyl ether(AME),tenuazonic acid(TeA)and tentoxin(TEN)in maize,and to detect the background values of AOH,AME,TeA and TEN in 30 forage maize samples from Shandong Province. The maize sample was dissolved with water,extracted with 0.1% formic acid acetonitrile solution,salted out with sodium chloride,and Agilent EC-C18 column(100 mm×2.1 mm,2.7μm)for the test chromatographic column,the mobile phases A and B are eluted with acetonitrile phase and ultra-pure water phase gradient respectively,and the negative ion ionization mode(ESI-)is used as the ionization condition. The monitoring mode is multi reactive ion monitoring mode(MRM)for quantitative and qualitative analysis. The QuEChERS-UHPLC-MS/MS method was evaluated by standard curve,accuracy and precision tests for the detection of Alternaria toxins. The results showed that the linear relationship was good in the range of 1 to 100μg/L of the four Alternaria toxins,the spiked recoveries of TeA,AOH,AME and TEN were 74.70% to 84.60%,77.94% to 103.84%,72.61% to 102.14% and 71.16% to 73.16%,and the relative standard deviation(RSD)were 4.08% to 8.36%,2.03% to 4.07%,1.80% to 4.61% and 1.99% to 2.40%,respectively. The method was used to assay 30 forage maize samples from Shandong Province,no TEN was detected and the positive rates of AOH,AME and TeA were 96.67%,93.30%,40.00%,respectively. In conclusion,the QuEChERS-UHPLC-MS/MS method which we established in this experiment had high accuracy and precision,good stability,and can be used as a method for the determination of AOH,AME,TeA and TEN in maize. The positive rates of AOH,AME and TeA of forage maize samples from Shandong Province are higher,close attention should be paid to it.[Chinese Journal of Animal Nutrition,2023,35(1):643-651]
作者
张环宇
朱连勤
陈甫
王倩文
朱风华
马向东
李艳召
ZHANG Huanyu;ZHU Lianqin;CHEN Fu;WANG Qianwen;ZHU Fenghua;MA Xiangdong;LI Yanzhao(College of Veterinary Medicine,Qingdao Agricultural University,Qingdao 266109,China;College of Animal Science and Technology,Qingdao Agricultural University,Qingdao 266109,China;Qingdao Vland Biotech Group Co.,Ltd.,Qingdao 266102,China;Rejing(Langfang)Biotechnology Co.,Ltd.,Langfang 065000,China)
出处
《动物营养学报》
CAS
CSCD
北大核心
2023年第1期643-651,共9页
CHINESE JOURNAL OF ANIMAL NUTRITION
基金
山东省羊产业技术体系营养与饲料岗位(SDAIT-10-04)
山东省家禽产业技术体系营养与饲料岗位(SDAIT-11-07)。
