超高效液相色谱-串联质谱法测定虾干中12种工业染料
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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 C_(18)(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.
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 C_(18)(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.
引文
[1] 罗诗萌, 赵建忠, 于秋红, 等. 豆制品中15种工业染料的超快速液相色谱串联四级杆质谱快速筛查法[J]. 职业与健康, 2014, 30(8): 1052-1055.
[2] 冯月超, 贾丽, 何亚荟, 等. 超高效液相色谱-串联质谱法同时测定粮食及肉制品中的24种工业染料[J]. 色谱, 2013, 31(10): 1021-1027.
[3] 张春玲, 蒲彦利, 王红波, 等. 高效液相色谱法测定薯片中9种工业染料[J]. 中国卫生检验杂志, 2017, 27(21): 3077-3079.
[4] 刘瀚升. 高效液相色谱法同时测定熟肉制品中的罗丹明B、苏丹红Ⅰ、Ⅱ、Ⅲ、Ⅳ、碱性橙2、21、22、酸性橙Ⅱ和红2G[J]. 实用预防医学, 2016, 23(1): 108-110.
[5] 胡海山, 鄢兵, 张云伟. 凝胶色谱净化超高效液相色谱法测定食品中10种工业染料[J]. 分析科学学报, 2017, 33(3): 362-366.
[6] 路杨, 杨立新, 刘印平, 等. 凝胶渗透色谱净化超高效液相色谱法测定辣椒油和火锅底料中的10种工业染料[J]. 食品安全质量检测学报, 2015, 6(2): 647-652.
[7] 杨毅华, 徐明敏, 陈波, 等. 实验技术与方法固相萃取-反相高效液相色谱法同时测定葡萄干中5种工业染料[J]. 中国食品卫生杂志, 2016, 28(1): 52-55.
[8] 李兰, 刘俊, 王丰. 高效液相色谱-二极管阵列检测器法测定胶囊壳中20种禁用工业染料[J]. 分析化学, 2016, 44(7): 1112-1118.
[9] 邵国健, 朱文涛, 韩建康. 超高效液相色谱-串联质谱法同时测定膨化食品中10种工业染料[J]. 中国卫生检验杂志, 2017, 27(6): 784-788.
[10] 赵珊, 张晶, 丁晓静, 等. 超高效液相色谱电喷雾串联四极杆质谱法检测豆制品中12种禁用工业染料[J]. 分析测试学报, 2016, 35(4): 432-437.
[11] 顾万江, 胡黎黎, 唐晓琴. 超高效液相色谱-四极杆-静电场轨道阱高分辨质谱法快速筛查食品中9种工业染料[J]. 中国卫生检验杂志, 2018, 28(1): 13-17.
[12] 陈林, 温家欣, 吴霞, 等. 改良QuEChERS技术结合液相色谱-串联质谱联用法同时快速检测辣椒制品中14种非法添加工业染料[J]. 食品科学, 2017, 38(8): 296-302.
[13] 宋鑫, 杭学宇, 王露, 等. 全自动凝胶渗透色谱-固相萃取联合净化-超高效液相色谱-串联质谱法测定肉类制品中8种工业染料[J]. 理化检验:化学分册, 2016, 52(6): 725-728.
[14] 林子豪, 戚平, 周庆琼, 等. 液相色谱-串联质谱内标法同时测定调味品中11种工业染料[J]. 现代食品科技, 2017, 33(7): 301-307.
[15] 罗诗萌, 于秋红, 牛晓梅,等.UFLC-MS-MS方法快速筛查葡萄酒和辣椒中的17种工业染料 [J]. 中国卫生检验杂志, 2014, 24(6): 819-823.
[2] 冯月超, 贾丽, 何亚荟, 等. 超高效液相色谱-串联质谱法同时测定粮食及肉制品中的24种工业染料[J]. 色谱, 2013, 31(10): 1021-1027.
[3] 张春玲, 蒲彦利, 王红波, 等. 高效液相色谱法测定薯片中9种工业染料[J]. 中国卫生检验杂志, 2017, 27(21): 3077-3079.
[4] 刘瀚升. 高效液相色谱法同时测定熟肉制品中的罗丹明B、苏丹红Ⅰ、Ⅱ、Ⅲ、Ⅳ、碱性橙2、21、22、酸性橙Ⅱ和红2G[J]. 实用预防医学, 2016, 23(1): 108-110.
[5] 胡海山, 鄢兵, 张云伟. 凝胶色谱净化超高效液相色谱法测定食品中10种工业染料[J]. 分析科学学报, 2017, 33(3): 362-366.
[6] 路杨, 杨立新, 刘印平, 等. 凝胶渗透色谱净化超高效液相色谱法测定辣椒油和火锅底料中的10种工业染料[J]. 食品安全质量检测学报, 2015, 6(2): 647-652.
[7] 杨毅华, 徐明敏, 陈波, 等. 实验技术与方法固相萃取-反相高效液相色谱法同时测定葡萄干中5种工业染料[J]. 中国食品卫生杂志, 2016, 28(1): 52-55.
[8] 李兰, 刘俊, 王丰. 高效液相色谱-二极管阵列检测器法测定胶囊壳中20种禁用工业染料[J]. 分析化学, 2016, 44(7): 1112-1118.
[9] 邵国健, 朱文涛, 韩建康. 超高效液相色谱-串联质谱法同时测定膨化食品中10种工业染料[J]. 中国卫生检验杂志, 2017, 27(6): 784-788.
[10] 赵珊, 张晶, 丁晓静, 等. 超高效液相色谱电喷雾串联四极杆质谱法检测豆制品中12种禁用工业染料[J]. 分析测试学报, 2016, 35(4): 432-437.
[11] 顾万江, 胡黎黎, 唐晓琴. 超高效液相色谱-四极杆-静电场轨道阱高分辨质谱法快速筛查食品中9种工业染料[J]. 中国卫生检验杂志, 2018, 28(1): 13-17.
[12] 陈林, 温家欣, 吴霞, 等. 改良QuEChERS技术结合液相色谱-串联质谱联用法同时快速检测辣椒制品中14种非法添加工业染料[J]. 食品科学, 2017, 38(8): 296-302.
[13] 宋鑫, 杭学宇, 王露, 等. 全自动凝胶渗透色谱-固相萃取联合净化-超高效液相色谱-串联质谱法测定肉类制品中8种工业染料[J]. 理化检验:化学分册, 2016, 52(6): 725-728.
[14] 林子豪, 戚平, 周庆琼, 等. 液相色谱-串联质谱内标法同时测定调味品中11种工业染料[J]. 现代食品科技, 2017, 33(7): 301-307.
[15] 罗诗萌, 于秋红, 牛晓梅,等.UFLC-MS-MS方法快速筛查葡萄酒和辣椒中的17种工业染料 [J]. 中国卫生检验杂志, 2014, 24(6): 819-823.