磁性氧化石墨烯固相萃取-高效液相色谱串联质谱法测定花生中黄曲霉毒素的含量
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摘要
建立了磁固相萃取-高效液相色谱串联质谱(MSPE-HPLC-MS/MS)测定花生黄曲霉毒素的确证性检测方法,利用甲醇-水溶液对样品进行提取,使用磁性固相萃取材料萃取、富集和净化样品初提液中的黄曲霉毒素,高效液相色谱串联质谱定量检测。对影响磁性固相萃取效率的条件进行了优化,主要包括吸附剂用量、萃取溶剂浓度、萃取时间、洗脱剂选择、洗脱周期等。结果表明,黄曲霉毒素在其线性范围内线性关系良好,相关系数均大于0. 998 2,回收率为91. 0%～120. 2%,相对标准偏差为1. 1%～5. 6%,检出限为0. 01～0. 04μg/kg。该方法样品富集净化操作简单、准确可靠、检出限低,能够满足花生样品黄曲霉毒素的检测。
A method for the determination of Aflatoxins in peanuts by magnetic solid phase extraction-high performance liquid chromatography-triple quadrupole mass spectrometry( MSPE-HPLC-MS/MS) was developed.Firstly,peanut sample was extracted with methanol-water,and then the extraction solvent was enriched and purified by magnetic solid phase extraction materials.Aflatoxins were analyzed by HPLC-MS/MS. Several parameters,which could affect the extraction efficiency including materials amount,methanol concentration,extraction time,eluent solvent selection and elution cycle were optimized accordingly. Under the optimized conditions,the linear relationships were good and the correlation coefficients were greater than 0. 998 2.The recovery of Aflatoxins ranging from 91. 0% ～ 120. 2%,and the relative standard deviations between 1. 1% ～ 5. 6%,the limit of detection were0. 01 ～ 0. 04 μg/kg. This method was simple,accurate and reliable for the detection and purification with good detection limit,which could be applied to the routine analyze of Aflatoxins in peanuts.
A method for the determination of Aflatoxins in peanuts by magnetic solid phase extraction-high performance liquid chromatography-triple quadrupole mass spectrometry( MSPE-HPLC-MS/MS) was developed.Firstly,peanut sample was extracted with methanol-water,and then the extraction solvent was enriched and purified by magnetic solid phase extraction materials.Aflatoxins were analyzed by HPLC-MS/MS. Several parameters,which could affect the extraction efficiency including materials amount,methanol concentration,extraction time,eluent solvent selection and elution cycle were optimized accordingly. Under the optimized conditions,the linear relationships were good and the correlation coefficients were greater than 0. 998 2.The recovery of Aflatoxins ranging from 91. 0% ～ 120. 2%,and the relative standard deviations between 1. 1% ～ 5. 6%,the limit of detection were0. 01 ～ 0. 04 μg/kg. This method was simple,accurate and reliable for the detection and purification with good detection limit,which could be applied to the routine analyze of Aflatoxins in peanuts.
引文
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[10]彭茂民,刘丽,王小飞,等.免疫亲和柱净化-HPLC法测定小麦粉中的黄曲霉毒素B1、玉米赤霉烯酮和脱氧雪腐镰刀菌烯醇的含量[J].食品科技,2017,42(9):305-308.
[11]王青,徐美蓉,黄铮,等.磁性固相萃取技术在食品安全检测中的应用进展[J].甘肃农业科技,2018,43(8):17-20.
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[13]陈林吉,朱晁乐,曹小吉,等.磁性氮掺杂石墨烯固相萃取环境水样中的4种有机氯污染物[J].分析化学,2017,45(5):762-769.
[14]李燕莹,周庆琼,陈羽中,等.磁固相萃取在食品分析中的研究进展[J/OL].食品工业科技. http://kns.cnki.net/kcms/detail/11. 1759. TS. 20181116. 1031. 004.html.
[15]何晓明,赵月钧,倪娟桢,等.β-环糊精磁性石墨烯固相萃取-高效液相色谱-串联质谱法测定瓜果中的9种植物生长调节剂残留量[J].食品科技,2018,43(10):345-351.
[16]郭宇彤,李欣悦,高仕谦,等.磁性氧化石墨烯固相萃取/高效液相色谱-串联质谱法测定环境水样中6种三嗪类除草剂残留[J].分析测试学报,2016,35(11):1 384-1 389.
[17]喻理,李培武,杨代斌,等.一种磁性石墨烯复合材料及其制备方法和应用:108 722 350A[P].2018-11-02.
[18]王秀嫔,李培武,杨扬,等.液相色谱-三重串联四极杆质谱测定粮油中的黄曲霉毒素[J].色谱,2011,29(6):517-522.
[2]ARDIC M,KARAKAYA Y,ATASEVER M,et al.Determination of Aflatoxin B1levels in deep-red ground pepper(isot)using immunoaffinity column combined with ELISA[J]. Food Chem. Toxicol.,2008,46(5):1 596-1 599.
[3]DING X X,LI P W,BAI Y Z,et al.Aflatoxin B1in postharvest peanuts and dietary risk in China[J]. Food Control,2012,23(1):143-148.
[4]NEAGU D,CAPODILUPO A,VILKANAUSKYTE A,et al.AFB1-AP conjugate for enzyme immunoassay of Aflatoxin B1in corn samples[J]. Anal. Lett.,2009,42(8):1 170-1 186.
[5]ZHANG D H,LI P W,YANG Y,et al.A high selective immunochromatographic assay for rapid detection of Aflatoxin B1[J].Talanta,2011,85(1):736-742.
[6]COMMISSION REGULATION(EC). Setting maximum levels for certain contaminants in foodstuffs:No 165/2010[S].2010.
[7]国家食品药品监督管理总局.食品安全国家标准食品中真菌毒素限量:GB 2761—2017[S].2017.
[8]杨琳,张宇昊,马良.高效液相色谱法同时检测粮谷中的黄曲霉毒素和赭曲霉毒素[J].食品科学,2010,31(24):250-254.
[9]宋月,陈颖,白欣.光化学衍生-高效液相色谱法检测食品中的黄曲霉毒素[J].实用预防医学,2016,23(7):882-884.
[10]彭茂民,刘丽,王小飞,等.免疫亲和柱净化-HPLC法测定小麦粉中的黄曲霉毒素B1、玉米赤霉烯酮和脱氧雪腐镰刀菌烯醇的含量[J].食品科技,2017,42(9):305-308.
[11]王青,徐美蓉,黄铮,等.磁性固相萃取技术在食品安全检测中的应用进展[J].甘肃农业科技,2018,43(8):17-20.
[12]GEIM A K,NOVOSELOV K S.The rise of graphene[J].Nat.Mater.,2007,6(3):183-191.
[13]陈林吉,朱晁乐,曹小吉,等.磁性氮掺杂石墨烯固相萃取环境水样中的4种有机氯污染物[J].分析化学,2017,45(5):762-769.
[14]李燕莹,周庆琼,陈羽中,等.磁固相萃取在食品分析中的研究进展[J/OL].食品工业科技. http://kns.cnki.net/kcms/detail/11. 1759. TS. 20181116. 1031. 004.html.
[15]何晓明,赵月钧,倪娟桢,等.β-环糊精磁性石墨烯固相萃取-高效液相色谱-串联质谱法测定瓜果中的9种植物生长调节剂残留量[J].食品科技,2018,43(10):345-351.
[16]郭宇彤,李欣悦,高仕谦,等.磁性氧化石墨烯固相萃取/高效液相色谱-串联质谱法测定环境水样中6种三嗪类除草剂残留[J].分析测试学报,2016,35(11):1 384-1 389.
[17]喻理,李培武,杨代斌,等.一种磁性石墨烯复合材料及其制备方法和应用:108 722 350A[P].2018-11-02.
[18]王秀嫔,李培武,杨扬,等.液相色谱-三重串联四极杆质谱测定粮油中的黄曲霉毒素[J].色谱,2011,29(6):517-522.