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UPLC-MS/MS法同时测定蛋白饮料和液体调味品中36种防腐剂OACSTPCD

Simultaneous determination of 36 preservatives in protein drinks and liquid condiments by UPLC-MS/MS

中文摘要英文摘要

采用提取和净化相结合的前处理方式,建立并优化了同时测定蛋白饮料、液体调味品中36种防腐剂的超高效液相色谱-串联质谱检测方法.样品采用饱和NaCl溶液(用磷酸调节pH=3)净化和乙腈-甲醇(9∶1,体积比)(含体积分数为0.2%的甲酸)提取.采用C18反向色谱柱进行分离,以甲醇和5 mmol/L乙酸铵为流动相梯度洗脱,采用电喷雾离子源正负离子同时扫描,动态多反应监测模式,基质匹配标准曲线,外标法定量.结果表明,36种防腐剂在1~250 ng/mL线性良好(相关系数≥0.999),方法定量限为0.04~0.2 mg/kg;空白样品不同加标水平下的平均加标回收率为75%~119%;相对标准偏差为0.90%~9.8%.建立的高通量检测方法灵敏、快速,准确度高,操作简便且能有效减少基质干扰、降低检测成本,极大提高多种防腐剂的定性定量检测效率.

An ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometry(UPLC-MS/MS)method was developed and optimized for the simultaneous determination of 36 preservatives in protein drinks and liquid condiments by the pretreat-ment method of combining extraction and purification.The samples were purified with saturated sodium chloride solution(adjusting pH to 3 with phosphoric acid)and extracted with acetonitrile-methanol(9∶1,volume ratio)(containing 0.2%formic acid).The analytes were separated on a C18 chromatographic column using gradient elution with methanol-5 mmol/L ammonium acetate as the mobile phase,detec-ted by MS/MS in both positive ion and negative ion mode using dynamic multiple reaction monitoring,and finally quantified by the matrix-matched external standard method.Results showed that good linearity was observed for the 36 compounds with correlation coefficients≥0.999 in the concentration range of 1-250 ng/mL,and the limits of quantitation were between 0.04 mg/kg and 0.2 mg/kg.The average recoveries of blank samples were in the range of 75%-119%,with relative standard deviations of 0.90%-9.8%.The established high-throughput detection method is sensitive,rapid,accurate,and simple,can effectively reduce matrix interference,reduce detection cost,shorten the detection cycle,and greatly improve the qualitative and quantitative detection efficiency of various preservatives.

魏宇涛;温泉;唐维英;黄璐瑶;余晓琴;杜钢;李澍才;李航

四川省食品检验研究院,四川成都,611731||国家市场监管重点实验室(白酒监管技术),四川成都,611731四川省药品检验研究院,四川成都,611731

防腐剂;蛋白饮料;液体调味品;超高效液相色谱串联质谱;动态多反应监测

preservatives;protein drinks;liquid condiments;ultra-high performance liquid chromatography-tandem mass spectrometry;dynamic multiple reaction monitoring

《食品与发酵工业》 2024 (001)

279-285 / 7

四川省市场监督管理局科技计划项目(SCSJS2022002)

10.13995/j.cnki.11-1802/ts.034884

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