超高效液相色谱-三重四极杆质谱法测定固体山楂制品中的展青霉素

Determination of patulin in hawthorn products by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  展青霉素  超高效液相色谱-三重四极杆质谱法  山楂制品

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

中文摘要:

      目的 建立超高效液相色谱-三重四极杆质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)检测固体山楂制品中展青霉素的含量。方法 样品经粉碎酶解后, 用乙酸乙酯提取, 阴离子交换柱净化浓缩, 以乙腈和水作为流动相进行梯度洗脱, 采用电喷雾离子源负模式测定, 同位素内标法定量。对前处理中复溶溶液、淋洗液、洗脱液进行优化, 并对优化后的方法进行方法学的验证。结果 展青霉素在5~100 μg/L浓度范围内线性良好, 相关系数大于0.999。在不同基质不同加标浓度下, 回收率93.4%~102.2%, 相对标准偏差小于3.5%。展青霉素在固体山楂片中的检出限为2 μg/kg, 定量限为5 μg/kg。结论 该方法准确可靠, 灵敏度高, 适用于固体山楂制品中展青霉素的测定。

英文摘要:

      Objective To develop a method for the determination of patulin in hawthorn products by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The solid samples were primarily hydrolyzed with pectinase, then extracted with ethyl acetate and concentrated, purified and enriched with ProElut PXA. The gradient elution was carried out with acetonitrile and water as mobile phase, the negative mode was determined by electrospray negative ionization (ESI-), and the internal standard method was used for quantitative analysis. The pretreatment method was optimized. The complex solution, leacheate and eluent were optimized, and the optimized method was validated by methodology. Results The calibration curve showed a good linearity in the range of 5-100 μg/L with the correlation coefficient more than 0.999. The recoveries were in the range of 93.4%-102.2% at spiked levels in different matrix and the relative standard deviations were less than 3.5%. The limit of detection was 2 μg/kg and the limit of quantitation was 5 μg/kg. Conclusion This method is reliable, accurate and sensitive, which can be used for the determination of patulin in hawthorn products.