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超高效液相色谱-串联质谱法测定蜂王浆中糠氨酸

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应用超高效液相色谱-串联质谱法建立一种适用于蜂王浆中糠氨酸含量的分析方法.样品用10.6 mol/L盐酸在110℃条件下水解24h,水解后的样品经C18固相萃取柱净化,3 mol/L盐酸洗脱,纯净水1∶1稀释,以2 mM甲酸铵水溶液(含0.01%甲酸)和2mM甲酸铵甲醇溶液(含0.01%甲酸)为流动相进行梯度洗脱,ACQUITY BEH C18柱上分离,电喷雾离子源(ESI)正离子模式,多反应监测模式(MRM)检测基质匹配,外标法定量.结果显示,糠氨酸在0.001 25~0.075 00mg/L范围内线性关系良好,相关系数(r2)为0.997,方法检出限(LOD)和定量限(LOQ)分别为17µg/kg和50μg/kg.在1倍、2倍和10倍LOQ这3个添加水平下,糠氨酸的平均回收率范围为105.8%~119.4%,相对标准偏差(RSD)为0.4%~4.9%(n=6).采用本方法对20批蜂王浆中的糠氨酸进行了测定,样品中糠氨酸含量在68.0~311.5 μg/kg之间.本方法检出限低、灵敏度高、准确性好,适用于蜂王浆中糠氨酸的测定.
Determination of furosine in royal jelly by ultra-performance liquid chromatography-tandem mass spectrometry
A method for the determination of furosine in royal jelly was developed using ultra performance liquid chromatog-raphy-tandem mass spectrometry.The sample was hydrolyzed with 10.6 mol/L hydrochloric acid at 110℃ for 24 h.Subse-quently,the hydrolyzed sample was purified using a C18 solid phase extraction column and eluted with 3 mol/L hydrochloric acid,followed by dilution in a 1∶1 ratio with pure water.Gradient elution was performed using mobile phases consisting of a 2 mM ammonium formate aqueous solution(containing 0.01%formic acid)and a 2 mM ammonium formate methanol so-lution(containing 0.01%formic acid)on a ACQUITY BEH C18 column.Detected in electrospray positive ionization mode with multiple reaction monitoring(MRM)mode and quantified by matrix matching curve external standard method.The re-sults demonstrated that furosine exhibited excellent linearity within the concentration range of 0.001 25-0.075 00 mg/L,with a correlation coefficient(r2)value of 0.997.The limits of detection(LOD)and quantitation(LOQ)were determined to be as low as 17 μg/kg and 50 µg/kg,respectively.Furthermore,the average recovery rates of furosine at levels corresponding to one,two,and ten times LOQ ranged from 105.8%to 1.19.4%,accompanied by relative standard deviations(RSD)ranging from 0.4%to 4.9%(n=6).This method was successfully employed to determine the content of furosine in twenty batches of royal jelly samples which varied between 68.0 μg/kg and 311.5 µg/kg.The method has a low detection limit,high sensitivi-ty,good accuracy,and is suitable for the determination of furosines in royal jelly.

Royal jellyFurosineUltra-performance liquid chromatography tandem mass spectrometry

史孟杰、胡晓楠、谢瑜杰、崔宗岩、常巧英、仝凯旋、吴兴强、范春林、陈辉

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中国检验检疫科学研究院 北京 100176

天津市食品安全检测技术研究院

秦皇岛海关技术中心

蜂王浆 糠氨酸 超高效液相色谱-串联质谱法

2024

质量安全与检验检测
中国检验检疫科学研究院

质量安全与检验检测

影响因子:0.399
ISSN:2096-8876
年,卷(期):2024.34(4)