1. 浙江工业大学化学工程学院
2. 浙江省疾病预防与控制中心
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项瑜芝, 许娇娇, 蔡增轩, 等. 同位素稀释高效液相色谱-串联质谱法测定水果及其制品中的展青霉素[J]. 分析测试学报, 2016,35(1):54-60.
Determination of Patulin in Fruit Products by Isotope Dilution Combined with High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. 2016,35(1):54-60.
建立了同位素稀释高效液相色谱-串联质谱法对水果及其制品中的展青霉素进行测定。澄清果汁(浊汁、固液体及固体样品需用果胶酶酶解处理,乙酸乙酯提取浓缩后复溶)经混合型阴离子交换柱净化、富集后,采用Waters HSS T3柱(2.1 mm×100 mm,1.8 μm)以乙腈-水为流动相梯度洗脱,电喷雾离子源离子化,负离子多反应离子监测(MRM)模式检测,同位素稀释内标法定量。展青霉素在5~250 ng/mL浓度范围内线性关系良好,相关系数(r2)大于0.999,该方法在不同基质不同加标浓度下,回收率为90.6%~110.1%,相对标准偏差(RSD)为1.4%~3.9%,定量下限为5.0 μg/kg(苹果汁中定量下限为2.0 μg/kg)。该方法准确可靠、灵敏度高,适合于水果及其制品中展青霉素的测定,可满足我国GB 2761-2011对于水果制品、果蔬汁和酒类(仅限苹果和山楂)中展青霉素残留的检测要求。
A method was developed for the determination of patulin in fruit products by isotope dilution with high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS).The clear juice was directly purified and enriched with ProElut PXA.Besides,the cloud juice,solid liquid and solid samples were primarily hydrolyzed with pectinase,then extracted with ethyl acetate and concentrated,redissolved with acetic acid solution(pH 4.0),and purified and enriched with ProElut PXA.The chromatographic separation was performed on a Waters HSS T3 column(2.1 mm×100 mm,1.8 μm) by gradient elution with acetonitrile-water as mobile phase.The patulin was detected by MS with electrospray negative ionization(ESI) under multiple reaction monitoring(MRM) mode.Accurate determination was achieved using isotope as the internal standard.Results showed that the calibration curve of patulin was linear in the range of 5-250 ng/mL with correlation coefficients greater than 0.999.The limits of quantitation(LOQ) of this method were 2.0 μg/kg for apple juice and 5.0 μg/kg for apple wine and haw.The recoveries of patulin at low,medium and high spiked concentration levels were in the range of 90.6%-110.1% with relative standard deviations of 1.4%-3.9%.The proposed method was proved to be a practical method which could completely satisfy the standard requirement GB 2761-2011 for detection of patulin in fruit products including apple juice,apple wine and haw products.In conclusion,this method was reliable,accurate and sensitive,and could be used for the analysis of patulin in fruit products.
展青霉素高效液相色谱-串联质谱法同位素稀释法水果及其制品
patulinhigh performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS)isotope dilutionfruit products
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