固相萃取-超高效液相色谱-串联质谱法测定工业染料中芳香胺
UHPLC-MS/MS Determination of Aromatic Amines in Industrial Dyes by Solid Phase Extraction
摘 要
工业染料中的偶氮染料在柠檬酸缓冲液中用连二亚硫酸钠还原为芳香胺,所得芳香胺经ProElut AZO专用硅藻土柱提取,用乙醚洗脱,浓缩至近干后用甲醇定容。以UPLC BEH C18色谱柱为分离柱,以不同体积比混合的甲酸-水(0.1+99.9)溶液和甲醇为流动相梯度洗脱,采用电喷雾电离源正离子模式检测。方法的检出限(3S/N)在0.5~1.0 mg·kg-1之间。24种芳香胺的平均回收率在71.8%~96.5%之间,相对标准偏差(n=5)均小于8.0%。
固相萃取
芳香胺
工业染料
UHPLC-MS/MS
Solid phase extraction
Aromatic amines
Industrial dyes
Abstract
The azo dyes of industrial dyes were reduced by sodium hyposulfite to form aromatic amines, which were extracted by passing through ProElut AZO specified diatomite column. The aromatic amines were eluted from column with diethyl ether, and the eluate was evaporated to near-dryness and made up to 1 mL with methanol. ACQUITY UPLC BEH C18 (100 mm×2.1 mm, 1.7 μm) column was used as stationary phase, and a mixture of methanol and formic acid (0.1+99.9) solution with different ratio was used as mobile phase in gradient elution. ESI and mode of positive ion were adopted in MS/MS. Values of detection limit (3S/N) of the method were found in the range of 0.5-1.0 mg·kg-1. Values of average recovery of 24 aromatic amines were found in the range of 71.8%-96. 5% and RSD′s (n=5) found were less than 8.0%.
中图分类号 O657.63
所属栏目 工作简报
基金项目 江苏省质量技术监督局科技项目(KJ103735)
收稿日期 2012/11/17
修改稿日期
网络出版日期
作者单位点击查看
联系人作者陈妍(qys-0708@163.com)
备注陈妍(1965-),女,江苏宜兴人,高级工程师,硕士研究生,研究方向为分析化学。
引用该论文: CHEN Yan,LI Xing-gen,QIAN Hui,HUANG Yin-bo,QIAO Yong-sheng,WANG Ai-xia. UHPLC-MS/MS Determination of Aromatic Amines in Industrial Dyes by Solid Phase Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2013, 49(3): 297～302
陈妍,李兴根,钱辉,黄银波,乔勇升,王爱霞. 固相萃取-超高效液相色谱-串联质谱法测定工业染料中芳香胺[J]. 理化检验－化学分册, 2013, 49(3): 297～302
被引情况:
【1】孙多志,左莹,禄春强,韩陈,秦紫明, "液相色谱-串联质谱法测定复合塑料食品包装袋中的二氨基甲苯",理化检验－化学分册 52, 52-55(2016)
【2】满正印,王全林,李和生,沈坚,张爱芝, "超高效液相色谱-串联质谱法测定具色塑料餐具中33种初级芳香胺的残留量和迁移量",理化检验－化学分册 52, 1142-1149(2016)
【3】郭琳琳,刘博静,王洪敏,袁 华, "高效液相色谱法测定间硝基苯磺酸还原制备间氨基苯磺酸过程中的间氨基苯磺酸和间硝基苯磺酸",理化检验－化学分册 52, 792-796(2016)
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参考文献
【1】韩京,杨水平,张燮,等.电喷雾解吸电离质谱法测定纺织品中致癌性芳香胺［J］.岩矿测试, 2009,28(6):507-513.
【2】孙银峰,牛增元,叶曦雯,等.液相色谱/质谱法测定电气产品塑料部件中的初级芳香胺［J］.分析化学, 2009,37(6):861-866.
【3】GB 19601-2004染料产品中23种有害芳香胺的限量及测定［S］.
【4】GB18401-2010国家纺织产品基本安全技术规范［S］.
【5】秦书琴,谭巧娣,尚洪英,等.纺织品禁用偶氮染料薄层色谱分析方法［J］.印染, 1997(3):8-12.
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【7】CASAL S, MENDES E, FERNANDES J O, et al. Analysis of heterocyclic aromatic amines in foods by gas chromatography-mass spectrometry as their tert.-butyldimethylsiyl derivatives［J］. Journal of Chromatography A, 2004,1040(1):105-114.
【8】MEHMET A, SEVKET A. Simultaneous determination of aliphatic and aromatic amines in water and sediment samples by ion-pair extraction and gas chromatography-mass spectrometry［J］. J Chromatogr A, 2006,1129:88-94.
【9】龙梅,谢孟峡,刘媛.应用RP-HPLC对芳香胺定量分析方法的研究［J］.北京师范大学学报:自然科学版, 2000,36(1):77-81.
【10】王卉卉,牛增元,叶曦雯,等.染色纺织品与皮革制品中23种禁用偶氮染料的高效液相色谱法测定［J］.分析测试学报, 2009,28(8):944-948.
【11】李英,张焱,荆瑞俊,等.气相色谱-质谱法测定纺织品中的芳香胺化合物［J］.印染, 2006,32(3):40-42.
【12】张焱,李英,燕庭毅.涂料印花浆中芳香胺的气质联用法分离测定［J］.染整技术, 2006,29:41.
【13】MANJUSHA S, SUNIK K S, AMIT A, et al. Fast separation and sensitive detection of carcinogenic aromatic amines by reversed-phase μ-liquid chromatography coupled with electrochemical detection［J］. J Chromatogr A, 2005,1089:52-58.
【14】黄丽芳,李来生,刘超.高效液相色谱-质谱法测定废水中芳香胺类化合物［J］.分析科学学报, 2008,24(3):265-269.
【15】SARAH K M, XENIA T T, ANNIE F, et al. Specific determination of 20 primary aromatic amines in aqueous food simulants by liquid chromatography-electrospray ionization-tandem mass spectrometry［J］. Journal of Chromatography A, 2005,1091(1):40-50.
【16】GB/T 17592-2011纺织品 禁用偶氮染料的测定［S］.
【17】SN/T 1045.1-2010进出口染色纺织品和皮革制品中禁用偶氮染料的测定 第1部分:液相色谱法［S］.
【18】SN/T 1045.2-2010进出口染色纺织品和皮革制品中禁用偶氮染料的测定 第2部分:气相色谱质谱法［S］.
【19】SN/T 1045.3-2010进出口染色纺织品和皮革制品中禁用偶氮染料的测定 第3部分:气相色谱法［S］.
【2】孙银峰,牛增元,叶曦雯,等.液相色谱/质谱法测定电气产品塑料部件中的初级芳香胺［J］.分析化学, 2009,37(6):861-866.
【3】GB 19601-2004染料产品中23种有害芳香胺的限量及测定［S］.
【4】GB18401-2010国家纺织产品基本安全技术规范［S］.
【5】秦书琴,谭巧娣,尚洪英,等.纺织品禁用偶氮染料薄层色谱分析方法［J］.印染, 1997(3):8-12.
【6】彭家钢,王丹华,吴采樱.自制SPME涂层顶空萃取-气相色谱法分析废水中的芳香胺类化合物［J］.分析测试学报, 2004,23(3):18-18.
【7】CASAL S, MENDES E, FERNANDES J O, et al. Analysis of heterocyclic aromatic amines in foods by gas chromatography-mass spectrometry as their tert.-butyldimethylsiyl derivatives［J］. Journal of Chromatography A, 2004,1040(1):105-114.
【8】MEHMET A, SEVKET A. Simultaneous determination of aliphatic and aromatic amines in water and sediment samples by ion-pair extraction and gas chromatography-mass spectrometry［J］. J Chromatogr A, 2006,1129:88-94.
【9】龙梅,谢孟峡,刘媛.应用RP-HPLC对芳香胺定量分析方法的研究［J］.北京师范大学学报:自然科学版, 2000,36(1):77-81.
【10】王卉卉,牛增元,叶曦雯,等.染色纺织品与皮革制品中23种禁用偶氮染料的高效液相色谱法测定［J］.分析测试学报, 2009,28(8):944-948.
【11】李英,张焱,荆瑞俊,等.气相色谱-质谱法测定纺织品中的芳香胺化合物［J］.印染, 2006,32(3):40-42.
【12】张焱,李英,燕庭毅.涂料印花浆中芳香胺的气质联用法分离测定［J］.染整技术, 2006,29:41.
【13】MANJUSHA S, SUNIK K S, AMIT A, et al. Fast separation and sensitive detection of carcinogenic aromatic amines by reversed-phase μ-liquid chromatography coupled with electrochemical detection［J］. J Chromatogr A, 2005,1089:52-58.
【14】黄丽芳,李来生,刘超.高效液相色谱-质谱法测定废水中芳香胺类化合物［J］.分析科学学报, 2008,24(3):265-269.
【15】SARAH K M, XENIA T T, ANNIE F, et al. Specific determination of 20 primary aromatic amines in aqueous food simulants by liquid chromatography-electrospray ionization-tandem mass spectrometry［J］. Journal of Chromatography A, 2005,1091(1):40-50.
【16】GB/T 17592-2011纺织品 禁用偶氮染料的测定［S］.
【17】SN/T 1045.1-2010进出口染色纺织品和皮革制品中禁用偶氮染料的测定 第1部分:液相色谱法［S］.
【18】SN/T 1045.2-2010进出口染色纺织品和皮革制品中禁用偶氮染料的测定 第2部分:气相色谱质谱法［S］.
【19】SN/T 1045.3-2010进出口染色纺织品和皮革制品中禁用偶氮染料的测定 第3部分:气相色谱法［S］.
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