分子印迹固相萃取-高效液相色谱法测定果汁中的展青霉素
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摘要
建立了分子印迹固相萃取-高效液相色谱法测定果汁中展青霉素的方法。浓缩果汁样品经酶解,乙酸-水溶液稀释,分子印迹固相萃取小柱净化后(澄清果汁样品经乙酸-水溶液稀释后,直接进行SPE净化),以Waters XSELECT HSS T3色谱柱为分离柱,以水和乙腈作为流动相,二极管阵列检测器高效液相色谱进行检测,外标法定量。展青霉素在20～1000μg/L质量浓度范围内线性关系良好,相关系数为0.9994,方法的定量限为10.0μg/kg;添加水平为10.0、20.0μg/kg和40.0μg/kg时,加标回收率为83.0%～91.5%,相对标准偏差为2.8%～7.6%。结果表明:该方法准确、高效、特异性好、重现性高,适用于果汁中展青霉素的测定。
A method was developed for the determination of patulin in juice by molecularly imprinted solid phase extraction and high performance liquid chromatography. The cloudy juice was hydrolyzed by enzyme and diluted with acetic acid-water solution. The extract of cloudy juice was then enriched and purified by a molecularly imprinted solid-phase extraction(SPE) cartridge. If the juice was clear, it was diluted with acetic acid-water solution and then directly treated by the cartridge as above. The separation was perfoemed on a Waters XSELECT HSS T3 column with the mobile phase of acetonitrile and water.The patulin was detected by high performance liquid chromatography with diode array detector. External standard was used for the quantitative determination of patulin in juice. The good linearity was obtained in the range of 20～1000 μg/L with the correlation coefficient of 0.9994 and the limit of quantitation of 10.0 μg/kg. The average recoveries ranged from 83.0% to 91.5% at three spiked levels of 10.0, 20.0, 40.0 μg/kg with the relative standard deviations of 2.8%～7.6%. It was proved to be a accurate, efficient, specific and reproducible method which is suitable for the determination of patulin in juice.
A method was developed for the determination of patulin in juice by molecularly imprinted solid phase extraction and high performance liquid chromatography. The cloudy juice was hydrolyzed by enzyme and diluted with acetic acid-water solution. The extract of cloudy juice was then enriched and purified by a molecularly imprinted solid-phase extraction(SPE) cartridge. If the juice was clear, it was diluted with acetic acid-water solution and then directly treated by the cartridge as above. The separation was perfoemed on a Waters XSELECT HSS T3 column with the mobile phase of acetonitrile and water.The patulin was detected by high performance liquid chromatography with diode array detector. External standard was used for the quantitative determination of patulin in juice. The good linearity was obtained in the range of 20～1000 μg/L with the correlation coefficient of 0.9994 and the limit of quantitation of 10.0 μg/kg. The average recoveries ranged from 83.0% to 91.5% at three spiked levels of 10.0, 20.0, 40.0 μg/kg with the relative standard deviations of 2.8%～7.6%. It was proved to be a accurate, efficient, specific and reproducible method which is suitable for the determination of patulin in juice.
引文
[1]牛华,冯雷,牛之瑞,等.超高效液相色谱-串联质谱法测定果汁中的展青霉素[J].色谱,2012,30(9):957-961.
[2]Welke J E,Hoeltz M,Dottori H A,et al.Effict of processing stages of apple juice concentrate on patulin levels[J].Food control,2009,20(1):48-52.
[3]Martins M L,Gimeno A,Martins H M,et al.Cooccurrence of patulin and citrinin in Portuguese apples with rotten spots[J].Food additives&contaminants,2002,19(6):568-574.
[4]Al-Hazmi N A.Determination of Patulin and Ochratoxin A using HPLC in apple juice samples in Saudi Arabia[J].Saudi journal of biological sciences,2010,17(4):353-359.
[5]Cunha S C,Faria M A,Fernandes J O.Determination of patulin in apple and quince products by GC-MSusing 13C5-7 patulin as internal standard[J].Food chemistry,2009,115(1):352-359.
[6]Barreira M J,Alvito P C,Almeida C M M.Occurrence of patulin in apple-based-foods in Portugal[J].Food chemistry,2010,212(3):653-658.
[7]Boonzaaijer G,Bobeldijk I,Van Osenbruggen W A.Analysis of patulin in dutch food,an evaluation of a SPEbased method[J].Food control,2005,16(7):587-591.
[8]吕伟超,申书昌,王超.固相萃取-超高效液相色谱联用测定水果及果酱中的展青霉素[J].色谱,2017,35(11):1160-1164.
[9]王立亚,刘嘉飞,李星星,等.超高效液相色谱-三重四级杆质谱法测定固体山楂制品中的展青霉素[J].食品安全质量检测学报,2018,12(9):2975-2979.
[10]赵红磊,杨丽蓉,赵红艳.超高效液相色谱-质谱联用法(UFLC-MS/MS)测定山楂片中展青霉素含量的研究[J].生物技术世界,2016,(2):16-18.
[11]Marta V,Zbynek D,Ondrej L,et al.Monitoring survey of patulin in a variety of fruit-based products using a sensitive UHPLC-MS/MS analytical procedure[J].Food control,2015,47:577-584.
[12]Christensen H B,Poulsen M E,Rasmussen P H,et al.Development of an LC-MS/MS method for the determination of pesticides and patulin in apples[J].Food additives&contaminants,2009,26(7):1013-1023.
[13]马雪涛,谭建林,牛之瑞,等.分子印迹柱净化-UPLC-MS/MS测定果蔬制品中展青霉素[J].食品研究与开发,2016,37(23):134-137.
[14]邓鸣,朱斌,宾春燕.分子印迹固相萃取-高效液相色谱法测定中成药中展青霉素[J].中成药,2014,36(10):2224-2226.
[15]何庆华,许杨.分子印迹技术在真菌毒素检测中的应用[J].食品科学,2009,30(11):273-275.
[2]Welke J E,Hoeltz M,Dottori H A,et al.Effict of processing stages of apple juice concentrate on patulin levels[J].Food control,2009,20(1):48-52.
[3]Martins M L,Gimeno A,Martins H M,et al.Cooccurrence of patulin and citrinin in Portuguese apples with rotten spots[J].Food additives&contaminants,2002,19(6):568-574.
[4]Al-Hazmi N A.Determination of Patulin and Ochratoxin A using HPLC in apple juice samples in Saudi Arabia[J].Saudi journal of biological sciences,2010,17(4):353-359.
[5]Cunha S C,Faria M A,Fernandes J O.Determination of patulin in apple and quince products by GC-MSusing 13C5-7 patulin as internal standard[J].Food chemistry,2009,115(1):352-359.
[6]Barreira M J,Alvito P C,Almeida C M M.Occurrence of patulin in apple-based-foods in Portugal[J].Food chemistry,2010,212(3):653-658.
[7]Boonzaaijer G,Bobeldijk I,Van Osenbruggen W A.Analysis of patulin in dutch food,an evaluation of a SPEbased method[J].Food control,2005,16(7):587-591.
[8]吕伟超,申书昌,王超.固相萃取-超高效液相色谱联用测定水果及果酱中的展青霉素[J].色谱,2017,35(11):1160-1164.
[9]王立亚,刘嘉飞,李星星,等.超高效液相色谱-三重四级杆质谱法测定固体山楂制品中的展青霉素[J].食品安全质量检测学报,2018,12(9):2975-2979.
[10]赵红磊,杨丽蓉,赵红艳.超高效液相色谱-质谱联用法(UFLC-MS/MS)测定山楂片中展青霉素含量的研究[J].生物技术世界,2016,(2):16-18.
[11]Marta V,Zbynek D,Ondrej L,et al.Monitoring survey of patulin in a variety of fruit-based products using a sensitive UHPLC-MS/MS analytical procedure[J].Food control,2015,47:577-584.
[12]Christensen H B,Poulsen M E,Rasmussen P H,et al.Development of an LC-MS/MS method for the determination of pesticides and patulin in apples[J].Food additives&contaminants,2009,26(7):1013-1023.
[13]马雪涛,谭建林,牛之瑞,等.分子印迹柱净化-UPLC-MS/MS测定果蔬制品中展青霉素[J].食品研究与开发,2016,37(23):134-137.
[14]邓鸣,朱斌,宾春燕.分子印迹固相萃取-高效液相色谱法测定中成药中展青霉素[J].中成药,2014,36(10):2224-2226.
[15]何庆华,许杨.分子印迹技术在真菌毒素检测中的应用[J].食品科学,2009,30(11):273-275.