液相色谱法及液相色谱-串联质谱法测定山楂及其制品中展青霉素的结果比较与建议

目的比较液相色谱法(liquidchromatography,LC)和液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry, LC-MS/MS)测定山楂及其制品中展青霉素的方法学指标。方法 LC法:山楂及固体制品经粉碎酶解后,用乙酸乙酯提取,Mycosep?228Aflapat净化柱净化浓缩,以乙腈和水作为流动相进行梯度洗脱,液相色谱仪被测定; LC-MS/MS法:样品处理方法同LC法(除加同位素外),以乙腈和水作为流动相进行梯度洗脱,外标法定量,采用电喷雾离子源负模式测定。结果 LC法和LC-MS/MS法展青霉素在10～200 ng/mL浓度内线性良好,相关系数均大于0.9999; LC法的回收率为96.12%～104.20%, RSD均小于2.5%,检出限为0.52～0.63μg/kg,定量限为1.7～2.0μg/kg; LC-MS/MS法的回收率为94.68%～103.59%, RSD均小于2.5%,检出限为0.12～0.39μg/kg,定量限为0.38～1.29μg/kg。结论 2种方法结果无显著差异,均可适用于山楂及山楂制品中展青霉素的测定。

Comparison and suggestion of the determination of patulin in hawthorn and hawthorn products by liquid chromatography method and liquid phase-series mass spectrometry method

Objective To compare the methodological indexes of liquid chromatography (LC) and liquid phase-series mass spectrometry (LC-MS/MS) for determination of patulin in hawthorn and its products. Methods LC method: After enzymolysis by crushing, hawthorn and solid products were extracted by ethyl acetate, purified and concentrated by Mycosep?228 Aflapat purification column, gradient elution was conducted with acetonitrile and water as mobile phase, and the liquid chromatograph was measured. LC-MS/MS method: The sample treatment method was the same as LC method (except with isotopes), gradient elution was carried out with acetonitrile and water as mobile phase, quantitative determination was carried out with external standard method, and negative mode of electrospray ion source was adopted. Results Both the LC method and the LC-MS/MS method showed good linearities in the range of 10-200 ng/mL, and the correlation coefficients were greater than 0.9999. The recoveries of LC method were 96.12%?104.20%, RSDs were less than 2.5%, the limits of detection were 0.52?0.63 g/kg, and the limits of quantitation were 1.7?2.0 g/kg. The recoveries of LC-MS/MS were 94.68%?103.59%, the RSDs were less than 2.5%, the limits of detection were 0.12?0.39 g/kg, and the limits of quantitation were 0.38?1.29 g/kg. Conclusion There is no significant difference between the 2 methods, and both methods are suitable for the determination of patulin in hawthorn and hawthorn products.