固相萃取结合超高效液相色谱-串联质谱法快速测定乳粉及液体乳中26种吡咯里西啶生物碱的含量  

Rapid Determination of 26 Pyrrolizidine Alkaloids in Milk Power and Liquid Milk by Solid Phase Extraction Combined with Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：陈言凯 CHEN Yankai(National Quality Supervision and Testing Center for Processed Food,Fujian Inspection and Research Institute for Product Quality,Fuzhou 350002,China)

机构地区：[1]福建省产品质量检验研究院,国家加工食品质量检验检测中心,福建福州350002

出　　处：《食品科学》2024年第24期266-272,共7页Food Science

基　　金：福建省产品质量检验研究院科研项目(KY202220A);市场监管总局科技计划资助项目(2021MK054)。

摘　　要：以固相萃取结合超高效液相色谱-串联质谱技术,建立同时测定乳粉及液体乳中26种吡咯里西啶生物碱(pyrrolizidine alkaloids,PAs)含量的方法。样品采用5%三氯乙酸溶液进行提取、阳离子交换固相萃取柱净化后,经ACQUITY HSS T3色谱柱分离,以甲醇-0.1%甲酸溶液为流动相进行梯度洗脱,在电喷雾正离子源多反应监测模式下进行测定,采用外标法定量。在最优条件下进行方法验证,26种PAs化合物在1.0~40 ng/mL范围内线性关系良好,决定系数(R~2)均大于0.992,方法检出限(信噪比为3)为0.01~0.33μg/kg,定量限(信噪比为10)为0.03~1.0μg/kg。以空白乳粉和牛乳基质进行1、2、10倍定量限的加标回收实验(n=6),26种PAs化合物回收率在73.1%~111.6%之间,相对标准偏差为0.6%~9.8%。综上,该方法简单高效、灵敏度高、准确度好,适用于乳粉及液体乳中26种PAs的测定。A method was developed for the simultaneous determination of 26 pyrrolizidine alkaloids(PAs)in milk powder and liquid milk by solid phase extraction(SPE)combined with ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The samples were extracted with 5%trichloroacetic acid solution,cleaned up on a polymer cation exchange-solid phase extraction(PCX-SPE)column,separated on an ACQUITY HSS T3 column with gradient elution using a mobile phase consisting of methanol and 0.1%formic acid in water,detected using an electrospray ionization(ESI)in the positive ion mode with multiple reaction monitoring(MRM),and finally quantified by the external standard method.The method validation was performed under optimal conditions.The calibration curves for the 26 PA compounds showed good linearity in the range of 1.0–40 ng/mL with determination coefficients(R2)greater than 0.992.The limits of detection(LOD)and quantification(LOQ)of the developed method were in the range of 0.01-0.33μg/kg(RS/N=3)and 0.03–1.0μg/kg(RS/N=10),respectively.Recoveries for blank milk powder and liquid milk spiked at 1×,2×,and 10×LOQ levels ranged from 73.1%to 111.6%with relative standard deviations(RSDs,n=6)of 0.6%-9.8%.In conclusion,this method is simple,efficient,sensitive,accurate,and suitable for the determination of the 26 PAs in milk powder and liquid milk.

关 键 词：固相萃取 超高效液相色谱-串联质谱 乳粉和液体乳 吡咯里西啶生物碱 

分 类 号：TS207.3[轻工技术与工程—食品科学]