摘要
目的建立一种超高效液相色谱-串联质谱法同时测定虾干中12种工业染料(碱性橙2、碱性橙21、碱性橙22、碱性嫩黄O、碱性玫瑰精、结晶紫、苏丹红Ⅰ~Ⅳ、酸性橙2和酸性间黄胺)的定量分析方法。方法样品采用乙腈-水(3:1,V/V)超声提取,离心后取乙腈层进样分析;以5 mmol/L乙酸铵/0.1%甲酸-乙腈为流动相梯度洗脱,经ACQUITY UPLC BEH C_(18 )(2.1 mm×100 mm,1.7μm)柱分离后,采用多反应监测(MRM)模式检测。结果 12种染料的相关系数均>0.997,回收率为83.6%~118.0%,方法相对标准差<10%(n=6)。对20份虾干样品进行检测,12种工业染料均未检出。结论本法灵敏、简便,适用于虾干中12种工业染料的定量分析。
Objective To establish an ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for the determination of 12 industrial dyes(basic orange 2,basic orange 21,basic orange 22,auramine,Rhodamine B,crystal violet,Sudan red Ⅰ-Ⅳ,acid orange 2,metanil yellow)in dry shrimp.Methods Samples were extracted ultrasounically with acetonitrile-water(3:1,V/V)and then centrifuged.The acetonitrile layer was used for analysis.The separation was performed on ACQUITY UPLC BEH C18(2.1 mm×100 mm,1.7 μm)column with gradient elution of 0.1% formic acid in 5 mmol/L ammonium acetate solution and acetonitrile.The mass spectrometric acquisition was carried out under the mode of multiple reaction monitoring(MRM).Results The correlation coefficients were all greater than 0.997,the average recoveries were within 83.6%-118.0%,with relative standard deviations(RSD,n=6)less than 10%.20 dry shrimp samples were tested by this method and no industrial dye was detected.Conclusion This established UPLC-MS/MS method is simple,effective,sensitive and suitable for the determination of 12 industrial dyes in dry shrimp.
作者
张海君
何微娜
倪承珠
郝伟
ZHANG Hai-jun;HE Wei-na;NI Cheng-zhu;HAO Wei(Taizhou Center for Disease Control and Prevention,Taizhou,Zhejiang 318000,China)
出处
《中国卫生检验杂志》
CAS
2019年第6期658-661,668,共5页
Chinese Journal of Health Laboratory Technology
基金
浙江省台州市医药卫生科技项目(162yw08)
关键词
工业染料
超高效液相色谱-质谱联用法
虾干
Industrial dyes
Ultra performance liquid chromatography-tandem mass spectrometry
Dry shrimp
作者简介
张海君(1976-),男,本科,主管技师,主要从事理化检验工作;通讯作者:郝伟,E-mail:40320231l@qq.com.