潘项捷, 张水锋, 盛华栋, 焦玉芬, 施元旭, 冯婷婷. Determination of Five Quaternary Ammonium Salts in Frozen Drinks by High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. 2020, 39(9): 1120-1125.
潘项捷, 张水锋, 盛华栋, 焦玉芬, 施元旭, 冯婷婷. Determination of Five Quaternary Ammonium Salts in Frozen Drinks by High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. 2020, 39(9): 1120-1125.DOI: doi:10.3969/j.issn.1004-4957.2020.09.009.
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。
Abstract
A high-performance liquid chromatography-tandem mass spectrometric(HPLC-MS/MS) method was developed for the rapid determination of five quaternary ammonium salts
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.