CAJ | 학술논문

利用超高效液相色谱-四极杆飞行时间质谱（ UPLC-Q-TOF MS）技术建立了水产品中28种酸性合成色素的快速检测方法。水产样品采用氨水-水-乙醇（2：1：7，v／v／v）溶液提取，经氨基化吸附剂基质分散法净化后直接用UPLC-Q-TOF MS测定。目标物经 Eclipse Plus-C18柱分离，以0.1％（ v／v）甲酸-5 mmol／L乙酸铵水溶液和乙腈为流动相进行梯度洗脱，采用电喷雾负离子模式下全信息串联质谱扫描模式进行检测。结果表明：水产品中28种酸性合成色素的定量限（ LOQ，S／N=10）为20~100μg／kg；并在各自的线性范围内线性关系良好（相关系数 r）≥0.991，峰面积的相对标准偏差（ n=6）均小于5.61％；在3个加标水平下的平均回收率为70.24％~106.47％，相对标准偏差为5.62％~9.65％（ n=6）。该方法快速简单、灵敏度高，适用于水产品中28种色素的快速筛查。
이용초고효액상색보-사겁간비행시간질보（ UPLC-Q-TOF MS）기술건립료수산품중28충산성합성색소적쾌속검측방법。수산양품채용안수-수-을순（2：1：7，v／v／v）용액제취，경안기화흡부제기질분산법정화후직접용UPLC-Q-TOF MS측정。목표물경 Eclipse Plus-C18주분리，이0.1％（ v／v）갑산-5 mmol／L을산안수용액화을정위류동상진행제도세탈，채용전분무부리자모식하전신식천련질보소묘모식진행검측。결과표명：수산품중28충산성합성색소적정량한（ LOQ，S／N=10）위20~100μg／kg；병재각자적선성범위내선성관계량호（상관계수 r）≥0.991，봉면적적상대표준편차（ n=6）균소우5.61％；재3개가표수평하적평균회수솔위70.24％~106.47％，상대표준편차위5.62％~9.65％（ n=6）。해방법쾌속간단、령민도고，괄용우수산품중28충색소적쾌속사사。
An analytical method was established for the simultaneous determination of 28 acidic artificial dyes in fishery products by ultra performance liquid chromatography coupled with qua-drupole-time of flight mass spectrometry( UPLC-Q-TOF MS). The analytes in fishery products were extracted with ethyl alcohol containing 20%( v/v)ammonia water and 10%( v/v)water. Then the extract solution was purified according to amination adsorbent matrix dispersion method. The compounds were separated by an Eclipse Plus-C 18 column with acetonitrile and 0. 1%(v/v)formic acid-5 mmol/L ammonium acetate solution as the mobile phases,and measured by UPLC-Q-TOF MS with electrospray ionization in negative mode. As a result,the limits of quantification( LOQs,S/N = 10 ) of the target compounds were 20-100 μg/kg in fishery products. The 28 analytes behaved linearly in wide-range with the correlation coeffi-cients more than 0. 991 as well as the relative standard deviations( RSDs)of the peak areas less than 5. 61%( n = 6 ). The average recoveries of the 28 analytes spiked at three levels were ranged from 70. 24% to 106. 47% with RSDs of 5. 62%-9. 65%( n= 6 ). This method can be applied to the analysis of the 28 acidic artificial dyes in fishery products due to its fastness ,sim-plicity and relatively high sensitivity.