April 2013 Chinese Journal of Chromatography 380 ~ A

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1 Vol. 31 No. 4 April 2013 Chinese Journal of Chromatography 380 ~ 385 DOI /SP. J * UHPLC-MS /MS BS EN ISO Eclipse XDB-C18 RRHD MRM 0. 2 mg /kg 70% ~ 120% μg /L n = 7 15% 30 mg /kg - O658 A Determination of carcinogenic aromatic amines derived from azo colorants in textiles and leather by ultra high performance liquid chromatography-tandem mass spectrometry WEN Yuyun 1 2 OU Yan 2 HE Mingchao 2 GONG Zhenbin 3* 1. College of Ocean and Earth Sciences Xiamen University Xiamen China 2. Fareast Testing & Technology Services Co. Ltd Quanzhou China 3. College of Environment and Ecology Xiamen University Xiamen China Abstract A rapid determination method was developed for the quantification and confirmation of 22 carcinogenic aromatic amines derived from azo colorants in textiles and leather by ultra high performance liquid chromatography-tandem electrospray ionization mass spectrometry UHPLC-MS /MS. The methods of EN for textiles and ISO for leather were adopted for sample pretreatment finally diluted with methanol. The target compounds were separated by an Eclipse XDB-C18 RRHD column and eluted with methanol and water in gradient and then determined by positive electrospray ionization mass spectrometry under multiple reaction monitoring MRM mode. The external standard method was used for the quantitative analysis. The separation conditions fragment voltages collision energies etc. were optimized. The limits of quantification LOQ were below 0. 2 mg /kg for different compounds matrix spike recoveries ranged from 70% to 120% at the spiked levels of and μg /L and the relative standard deviations RSDs were less than 15%. The proposed method is rapid sensitive accurate and selective. Key words ultra high performance liquid chromatography-tandem mass spectrometry UHPLC-MS / MS carcinogenic aromatic amines azo colorants textiles leather aromatic amines AAs *. Tel /Fax zbgong@ xmu. edu. cn. B

2 % 1 22 Dr. Ehrenstorfer 95% Zorbax Eclipse XDB-C18 RRHD 100 mm 2. 1 mm 1. 8 μm MeOH 0 ~ 2. 0 min 10% MeOH ~ % MeOH 2. 0 ~ 3. 3 min 30% MeOH 3. 3 ~ min 30% MeOH ~ 65% MeOH 7. 2 ~ 8. 0 min 65% MeOH ~ 100% MeOH 2. 0 μl GC 7 - GC-MS min 0. 5 ml /min 40 HPLC ESI + HPLC-MS L /min GC HPLC kpa 35 psi GC-MS HPLC-MS L /min V 500 V EN MRM 1 MS UHPLC-MS /MS 1. 0 g /L MRM 1. 4 UHPLC- BS EN MS /MS AAs ISO Sutthivaiyakit ml μm APCI 18 2 AAs AAs HPLC-MS /MS / / HPLC AAs / AAs M + H + / 22 UHPLC-MS /MS Agilent 1290 Agilent min Agilent JetStream Technologies AJS ESI MassHunter AAs 1 AAs mg /L LC /MS Merck AAs / / LC /MS Sigma M + H + HPLC Tedia Milli-Q MRM 20 g /20 ml Optimizer frag-

3 mentor collision energy CE MRM MRM 1 1 MRM Table 1 MRM conditions for target compounds No. Compound CAS No. t R /min Precursor ion m /z Fragmentor / V Product ion m /z 1 4-aminobiphenyl * benzidine * chloro-o-toluidine * naphthylamine * o-aminoazotoluene * amino-4-nitrotoluene * chloroaniline * diaminoanisole * '-methylenedianiline * '-dichlorobenzidine * '-dimethoxybenzidine * '-dimethylbenzidine * '-methylenedi-o-toluidine * methoxy-m-toluidine * '-methylene-bis- 2-chloro-aniline * '-oxydianiline * '-thiodianiline * o-toluidine * diaminotoluene * trimethylaniline * o-anisidine * aminoazobenzene * 17 * Quantitative ion. CE collision energy. CE /V mmol /L 0% 0. 01% LC-MS 0. 05% 0. 1% AAs ph M + H + AAs

4 4-383 Fig MRM MRM chromatogram of the 22 aromatic amines AAs 1. 0 mg /L The Nos. are corresponding to Table S / 10% N = AAs LOQ 100 μg /L μg /L 0. 2 mg /kg AAs 30 mg /kg X μg /L AAs Y BS EN GC-MS 2 22 Table 2 Linear relationships and instrument limits of quantification LOQ of the 22 compounds No. * Linear range / μg /L Regression equation r 2 LOQ / μg /L Y = X Y = X Y = 2. 2X Y = X Y = 66. 0X Y = 8. 8X Y = 9. 7X Y = 38. 1X Y = X Y = 47. 6X Y = X Y = X Y = X Y = X Y = 36. 0X Y = X Y = X Y = 2. 78X Y = X Y = 92. 0X Y = X Y = X * The Nos. are corresponding to Table 1. Y peak area X mass concentration μg /L. LC-MS /MS MRM ESI matrix effect ME AAs μg /L 5% ~ 90% μg /L 5 # 19 # % ~ 120% 3

5 % No. * Natural fiber cotton /% 500 μg /L 1000 μg /L 1500 μg /L 3 22 Table 3 Matrix spike recoveries of the 22 compounds Synthetic fiber dacron /% 500 μg /L 1000 μg /L 1500 μg /L Natural leather cow leather /% 500 μg /L 1000 μg /L 1500 μg /L * The Nos. are corresponding to Table GC-MS 3 E n Table 4 4 Analytical results of real positive samples Sample No. and type This method / mg /kg GC-MS method / mg /kg cloth /olive benzidine benzidine canvas /dark blue 3 3'-dimethoxybenzidine '-dimethoxybenzidine leather /navy benzidine benzidine UHPLC-MS /MS UHPLC-MS /MS 22 GC-MS 1 Robinson T McMullan G Marchant R et al. Bioresour Technol Skipper P L Kim M Y Sun H L P et al. Carcinogenesis BS EN ISO ISO GB /T Kataoka H. J Chromatogr A Hong X Y Wen Y Y Lin F et al. Journal of Instrumental Analysis

6 Kang S Y Zhang Q Bai H et al. Chinese Journal of Analytical Chemistry Wang H H Niu Z Y Ye X W et al. Journal of Instrumental A nalysis. 16 Han J Yang S P Zhang X et al. Rock and Mineral Analysis Ding J H He H X Lin H L et al. Chinese Journal of Analytical Chemistry Zhu Y Zhu Y Wang L L. Chinese Journal of Chromatography Sun Y F Niu Z Y Ye X W et al. Chinese Journal of Analytical Chemistry Sutthivaiyakit P Achatz S Lintelmann J et al. Anal Bioanal Chem Zhang Y Yang C D Yang L et al. Physical Testing and Chemical Analysis Part B Chemical Analysis Wu Z Z Ding J H Lai J H et al. Rock and Mineral Analysis Tang C J Nie J M Wang X N et al. Chinese Journal of Analysis Laboratory Yu H X. Advanced Measurement and Laboratory Management

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