Reduced graphene oxide and gold nanoparticle composite-based solid-phase extraction coupled with ultra-high-performance liquid chromatography-tandem mass spectrometry for the determination of 9 mycotoxins in milk

Reduced graphene oxide and gold nanoparticle composite-based solid-phase extraction coupled with ultra-high-performance liquid chromatography-tandem mass spectrometry for the determination of 9 mycotoxins in milk
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还原氧化石墨烯与纳米金颗粒复合固相萃取-超高效液相色谱-串联质谱法测定牛奶中9种霉菌毒素

DOI:
10.1016/j.foodchem.2018.05.041
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发表时间:
2018-10-30
期刊:
影响因子:
8.8
通讯作者:
Han, Zheng
Han, Zheng
中科院分区:
农林科学1区
文献类型:
--
作者:
Jiang, Keqiu;Huang, Qingwen;Han, Zheng

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以还原氧化石墨烯/纳米金(rGO/Au)复合物为固相萃取剂,对黄曲霉毒素B-1(AF B(1))、黄曲霉毒素M-1(AFM(1))、赭曲霉毒素A(OTA)、玉米赤霉烯酮(ZEA)、α-玉米赤霉烯醇(α-zearalenol在一些实施方案中,本发明涉及乳中的玉米赤霉烯醇(α-ZOL)、β-玉米赤霉烯醇(β-ZOL)、玉米赤霉酮(ZAN)、α-玉米赤霉醇(α-ZAL)和β-玉米赤霉醇(β-ZAL)。对影响固相萃取过程的主要参数进行了研究。结果表明,以2%乙腈水溶液为上样液,5%甲醇水溶液为洗脱液,甲醇/乙腈/甲酸(50/49/1,v/v/v)为洗脱剂,洗脱效果最佳。采用优化的样品前处理方法与超高效液相色谱-串联质谱联用检测,线性关系良好(R-2 >= 0.992),灵敏度高(定量限为0.02-0.18 ng/mL),回收率为70.2-111.2%,精密度为2.0-14.9%。在真实的牛奶样品中进一步验证了验证方法的适用性。
A reliable solid-phase extraction (SPE) procedure using reduced graphene oxide and gold nanoparticle (rGO/Au) composite as sorbent was proposed for purification and enrichment of aflatoxin B-1 (AFB(1)), aflatoxin M-1 (AFM(1)), ochratoxin A (OTA), zearalenone (ZEA), alpha-zearalenol (alpha-ZOL), beta-zearalenol (beta-ZOL), zearalanone (ZAN), alpha-zearalanol (alpha-ZAL) and beta-zearalanol (beta-ZAL) in milk. Main parameters affecting the performance of SPE procedure were thoroughly investigated. The optimized conditions included 2% acetonitrile in water as the loading solution, 5% methanol in water as the washing solution, and methanol/acetonitrile/formic acid (50/49/1, v/v/v) as the elution solvent. Satisfactory linearity (R-2 >= 0.992), high sensitivity (limit of quantification in the range of 0.02-0.18 ng mL(-1)), adequate recovery (70.2-111.2%), and acceptable precision (RSD, 2.0-14.9%) were obtained when the optimal sample pretreatment protocol was combined with ultra-high-performance liquid chromatography-tandem mass spectrometry detection. The applicability of the validated method was further verified in real milk samples.