| 高效液相色谱-串联质谱法测定冷冻饮品中的5种季铵盐 |
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| 基金项目:浙江省质量技术监督局科研计划项目(20180116) |
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| 中文摘要:建立了快速测定冷冻饮品中5种季铵盐(十二烷基二甲基苄基氯化铵、十四烷基二甲基苄基氯化铵、十六烷基二甲基苄基氯化铵、十六烷基二甲基苄基氯化铵、十二烷基三甲基氯化铵和双癸基二甲基氯化铵)的高效液相色谱-串联质谱(HPLC-MS/MS)检测方法。样品经乙腈-乙酸乙酯(1∶1，体积比)提取2次，提取液于-20 ℃冷冻脱脂净化，经CAPCELL PAK CR(1∶20)色谱柱分离，以乙腈-5 mmol/L乙酸铵(含0.1%甲酸)水溶液为流动相，梯度洗脱，采用多反应监测(MRM)模式，基质外标法进行定量分析。结果表明，5种季铵盐在0.5~50.0 μg/L质量浓度范围内线性关系良好，相关系数(r)均大于0.995。5种季铵盐的检出限为0.3~1.5 μg/kg，定量下限为1.0~5.0 μg/kg。样品基质在5.0、10.0和50.0 μg/kg 3个加标水平下的平均回收率为80.3%~114%，相对标准偏差(RSD)为2.5%~8.3%。实际样品检测结果表明，冷冻饮品中存在季铵盐的残留污染。该方法操作便捷，灵敏度高，精密度良好，适用于冷冻饮品中5种季铵盐的定量检测。 |
| 中文关键词:季铵盐 冷冻饮品 高相液相色谱-串联质谱法(HPLC-MS/MS) |
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| Determination of Five Quaternary Ammonium Salts in Frozen Drinks by High Performance Liquid Chromatography-Tandem Mass Spectrometry |
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| Abstract:A high-performance liquid chromatography-tandem mass spectrometric(HPLC-MS/MS) method was developed for the rapid determination of five quaternary ammonium salts,e.g.benzyldimethyldodecyl ammonium chloride，benzyldimethyltetradecyl ammonium chloride,benzyldimethylhexadecyl ammonium chloride,dodecyltrimethyl ammonium chloride,and didecyldimethyl ammonium chloride,in frozen drinks.The samples were extracted twice with acetonitrile-ethyl acetate(1∶1，by volume),then frozen to degrease at-20 ℃.The extract was separated on a CAPCELL PAK CR(1∶20) column using acetonitrile-5 mmoL ammonium acetate containing 0.1% formic acid as mobile phase by gradient elution.The target analytes were detected in multiple-reaction monitoring(MRM) mode,and quantified by the matrix matched external standard method.Results showed that good linearities for the five quaternary ammonium salts existed in the mass concentration range of 0.5-50.0 μg/L,with their correlation coefficients(r) larger than 0.995.The limits of detection(LOD) and limits of quantitation(LOQ) were in the ranges of 0.3-1.5 μg/kg and 1.0-5.0 μg/kg,respectively.The average recoveries for the five analytes at three spiked levels of 5.0,10.0 and 50.0 μg/kg ranged from 80.3% to 114% with relative standard deviations(RSD) of 2.5%-83%.With the advantages of convenient operation,high sensitivity and good precision,this method is suitable for the determination of five quaternary ammonium salts in frozen drinks. |
| Key Words:quaternary ammonium frozen drinks high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) |
| 引用本文：潘项捷，张水锋，盛华栋，焦玉芬，施元旭，冯婷婷.高效液相色谱-串联质谱法测定冷冻饮品中的5种季铵盐[J].分析测试学报,2020,39(9):1120-1125. |
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