同位素稀释超高效液相色谱-串联质谱法测定山楂及其口服液制品中的展青霉素

Determination of patulin in hawthorn and its oral solution products by isotope dilution combined with ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  展青霉素  超高效液相色谱-串联质谱法  同位素稀释法  山楂制品

英文关键词:patulin  ultra performance liquid chromatography-tandem mass spectrometry  isotope dilution  hawthorn products

中文摘要:

      目的 建立同位素稀释超高效液相色谱-串联质谱法测定山楂及其口服液制品中展青霉素含量的分析方法。方法 山楂样品需经粉碎、果胶酶酶解处理, 乙酸乙酯提取浓缩后复溶, 得到山楂样品溶液。山楂样品溶液和山楂口服液经多功能净化柱净化, 以乙腈-水为流动相梯度洗脱, 采用Agilent RRHD C18柱(2.1 mm× 100 mm, 1.8 μm), 电喷雾离子源负离子, 多反应离子监测模式检测, 同位素稀释内标法定量。结果 展青霉素在4.934~246.7 ng/mL浓度范围内线性关系良好, 相关系数r2大于0.999。在不同基质不同加标浓度下, 回收率为91.8%~105.4%, 相对标准偏差为1.8%~3.2%, 山楂检出限为3 μg/kg、定量限为10 μg/kg, 山楂口服液检出限为1.5 μg/kg、定量限为5 μg/kg。结论 该方法准确、可靠, 适用于山楂及其口服液制品中展青霉素的测定。

英文摘要:

      Objective To establish a method for the determination of patulin in hawthorn and its oral solution products by isotope dilution combined with ultra performance liquid chromatography-tandem mass spectrometry. Methods The hawthorn samples were crushed and hydrolyzed with pectinase, then extracted with ethyl acetate and concentrated, redissolved with acetic acid solution, and the hawthorn sample solution was obtained. The hawthorn sample solution and the oral solution of hawthorn were directly purified with multifunctional purification column. Agilent RRHD C18 column was used for gradient elution with acetonitrile-water as mobile phase. The patulin was detected by mass spectrometry with electrospray negative ionization (ESI﹣) under multiple reaction monitoring (MRM) mode. The isotope as internal standard method was used for quantitative analysis. Results The calibration curve was good linear in the range of 4.934?246.7 ng/mL with the correlation coefficients greater than 0.999. The recoveries were in the range of 91.8%?105.4% at low, medium and high spiked concentration levels in different matrix with relative standard deviations (RSDs) 1.8%~3.2%. The limits of detection (LOD) were 3 μg/kg for hawthorn and 1.5 μg/kg for oral solution of hawthorn. The limits of quantitation (LOQ) were 10 μg/kg for hawthorn and 5 μg/kg for oral solution of hawthorn. Conclusion This method is reliable, accurate, which can be used for the analysis of patulin in hawthorn and its oral solution products.