摘要
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,1.8μm)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/m L浓度范围内线性关系良好,相关系数(r^2)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5.0μg/kg(苹果汁中定量下限为2.0μg/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 dilu- tion 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 liq- uid 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 x 100 ram, 1.8 Ixm） by gradient elution with acetonitrile -water as mobile phase. The patulin was detec- ted 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 coeffi- cients 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 ap- ple juice, apple wine and haw products. In conclusion, this method was reliable, accurate and sen-sitive, and could be used for the analysis of patulin in fruit products.
出处
《分析测试学报》
CAS
CSCD
北大核心
2016年第1期54-60,共7页
Journal of Instrumental Analysis
关键词
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
patulin
high performance liquid chromatography tandem mass spectrometry （HPLC -MS/MS）
isotope dilution
fruit products
