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预防医学  2022, Vol. 34 Issue (6): 555-560    DOI: 10.19485/j.cnki.issn2096-5087.2022.06.003
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新鲜水果真菌毒素多组分检测方法研究
许娇娇, 蔡增轩, 王军淋, 徐美佳, 黄百芬
浙江省疾病预防控制中心理化与毒理检验所,浙江 杭州 310051
Development of an approach for simultaneous determination ofmulti-mycotoxins in fresh fruits
XU Jiaojiao, CAI Zengxuan, WANG Junlin, XU Meijia, HUANG Baifen
Department of Physicochemical and Toxicology, Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou, Zhejiang 310051, China
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摘要 目的 建立水果中真菌毒素多组分同时检测方法,为水果中真菌毒素监测提供技术支持。方法 采集市售新鲜水果样品,均质后称取2 g,加入10 mL乙腈-甲酸(体积比为99∶1)涡旋振荡10 min,加入1 g氯化钠和4 g无水硫酸钠提取,离心后取5 mL上清液,加入25 mg C18净化,离心取上清液氮气吹干,残渣用300 μL甲醇-乙腈(体积比为1∶1)复溶,700 μL去离子水混匀。采用液相色谱-串联质谱法(LC-MS/MS),以0.1%甲酸-5 mmol甲酸铵和甲醇-乙腈(体积比为1∶1)为流动相进行梯度洗脱,电喷雾离子源(ESI+/ESI-)、多反应监测模式(MRM)测定15种真菌毒素,基质匹配标准曲线定量。结果 15种真菌毒素在0.25~10 ng/mL浓度范围内线性关系良好,相关系数R2>0.992,方法检出限为0.1~1.0 μg/kg,加标回收率为71.68%~117.50%,相对标准偏差为0.01%~13.60%。检测市售新鲜水果203份,真菌毒素检出率为27.09%。结论 本研究优化后的LC-MS/MS法可同时检测新鲜水果中多种真菌毒素。
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许娇娇
蔡增轩
王军淋
徐美佳
黄百芬
关键词 真菌毒素液相色谱-串联质谱法新鲜水果    
AbstractObjective To develop an approach for simultaneous detection of multi-mycotoxins in fresh fruits, so as to provide technical supports for mycotoxins surveillance in fresh fruits. Methods Fresh fruits were collected from markets and homogenized. Then, 2 g of fresh fruits were added with 10 mL of 0.1% formic acid ( 99∶1, v/v ) in acetonitrile and wortexed for 10 min. Following extraction with 1 g of sodium chloride and 4 g of anhydrous sodium sulfate, samples were centrifuged and 5 mL of the supernatant was cleaned up with 25 mg C18. Following centrifugation, the supernatant was dried under nitrogen. The residue was dissolved in 300 μL of methanol-acetonitrile mixture solution ( 1∶1, v/v ), and mixed evenly in 700 μL of the distilled water. Samples were then eluted in gradient series of 0.1% formic acid and 5 mmol ammonium formate and methanol-acetonitrile mixture solution ( 1∶1, v/v ). The 15 mycotoxins were determined using liquid chromatography-tandem mass spectrometry ( LC-MS/MS ) with electrospray ion source (ESI+/ESI-) under multiple reaction monitoring. In addition, a matrix-matched standard curve was employed for quantitative analysis. Results There was a good linear relationship for 15 mycotoxins at concentrations of 0.25 to 10 ng/mL ( R2>0.992 ), the LC-MS/MS method showed the detection limits of 0.1-1.0 μg/kg, the spiked recovery rates of 71.68%-117.50%, and the relative standard deviations ( RSDs ) of 0.01%-13.60%. The detection rate of mycotoxins was 27.09% in 203 fresh fruits sold in markets. Conclusions The optimized LC-MS/MS method can be used for simultaneous determination of multi-mycotoxins in fresh fruits.
Key wordsmycotoxins    liquid chromatography-tandem mass spectrometry    fresh fruits
收稿日期: 2021-12-21      修回日期: 2022-03-22      出版日期: 2022-06-10
中图分类号:  R155.5  
基金资助:浙江省基础公益研究计划(LGC19H260001)
作者简介: 许娇娇,硕士,主管技师,主要从事食品安全理化检验工作
通信作者: 蔡增轩,E-mail:zxcai@cdc.zj.cn   
引用本文:   
许娇娇, 蔡增轩, 王军淋, 徐美佳, 黄百芬. 新鲜水果真菌毒素多组分检测方法研究[J]. 预防医学, 2022, 34(6): 555-560.
XU Jiaojiao, CAI Zengxuan, WANG Junlin, XU Meijia, HUANG Baifen. Development of an approach for simultaneous determination ofmulti-mycotoxins in fresh fruits. Preventive Medicine, 2022, 34(6): 555-560.
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http://www.zjyfyxzz.com/CN/10.19485/j.cnki.issn2096-5087.2022.06.003      或      http://www.zjyfyxzz.com/CN/Y2022/V34/I6/555
[1] ESKOLA M,KOS G,ELLIOTT C T,et al.Worldwide contamination of food-crops with mycotoxins:validity of the widely cited‘FAO estimate’of 25%[J].Crit Rev Food Sci Nutr,2022,60(16):2773-2789.
[2] WANG Y J,NIE J Y,YAN Z,et al.Multi-mycotoxin exposure and risk assessments for Chinese consumption of nuts and dried fruits[J].J Integr Agric,2018,17(7):1676-1690.
[3] SENGLING CEBIN COPPA C F,MOUSAVI KHANEGHAH A,ALVITO P,et al.The occurrence of mycotoxins in breast milk,fruit products and cereal-based infant formula:a review[J].Trends Food Sci Technol,2019,92:81-93.
[4] WANG Y J,NIE J Y,YAN Z,et al.Occurrence and co-occurrence of mycotoxins in nuts and dried fruits from China[J].Food Control,2018,88:181-189.
[5] ZHOU J,ZHANG D D,CHEN X H,et al.Investigation on the occurrence and contamination of multi-mycotoxin in chestnut and jujube(red date)[J/OL].J Chromatogr A,2021,1659(2021-08-23)[2022-03-22].https://doi.org/10.1016/j.chroma.2021.462486.
[6] AROUD H I,MAY B,DIETRICH H,et al.Influence of processing steps on the fate of ochratoxin A,patulin,and alternariol during production of cloudy and clear apple juices[J].Mycotoxin Res,2021,37(4):341-354.
[7] SADHASIVAM S,BARDA O,ZAKIN V,et al.Rapid detection and quantification of patulin and citrinin contamination in fruits[J/OL].Molecules,2021,26(15)(2021-07-27)[2022-03-22].https://doi.org/10.3390/molecules26154545.
[8] ZHOU J,XU J,CAI Z,et al.Simultaneous determination of five alternaria toxins in cereals using QuEChERS-based methodology[J].J Chromatogr B Analyt Technol Biomed Life Sci,2017,1068/1069:15-23.
[9] FAN Y Y,LIU F J,HE W Z,et al.Screening of multi-mycotoxins in fruits by ultra-performance liquid chromatography coupled to ion mobility quadrupole time-of-flight mass spectrometry[J/OL].Food Chem,2022,368(2021-08-13)[2022-03-22].https://doi.org/10.1016/j.foodchem.2021.130858.
[10] LAGO L O,NIEVIEROWSKI T H,MALLMANN L P,et al.QuEChERS-LC-QTOFMS for the simultaneous determination of legislated and emerging mycotoxins in malted barley and beer using matrix-matched calibration as a solution to the commercial unavailability of internal standards for some mycotoxins[J/OL].Food Chem,2021,345(2020-12-08)[2022-03-22].https://doi.org/10.1016/j.foodchem.2020.128744.
[11] 中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.合格评定化学分析方法确认和验证指南:GB/T 27417—2017[S].北京:中国标准出版社,2017.
General Administration of Quality Supervision, Inspection and Quarantine,Standardization Administration of the People's Republic of China.Comformity assessment-Guidance on validation and verification of chemical analytical methods:GB/T 27417-2017[S].Beijing:Standards Press of China,2017.
[12] European Commision.Commission Regulation(EU)No 519/2014 of 16 May 2014 amending Regulation(EC)No 401/2006 as regards methods of sampling of large lots,spices and food supplements,performance criteria for T-2,HT-2 toxin and citrinin and screening methods of analysis[J].Off J Eur Union,2014,147:29-43.
[13] JUAN C,MAÑES J,FONT G,et al.Determination of mycotoxins in fruit berry by-products using QuEChERS extraction method[J].LWT,2017,86:344-351.
[14] GUO W B,YANG J H,NIU X K,et al.A reliable and accurate UHPLC-MS/MS method for screening of Aspergillus,Penicillium and Alternaria mycotoxins in orange,grape and apple juices[J].Anal Methods,2021,13(2):192-201.
[15] ESCRIVÁ L,OUESLATI S,FONT G,et al.Alternaria mycotoxins in food and feed:an overview[J/OL].J Food Qual,2017[2022-03-22].https://doi.org/10.1155/2017/1569748.
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