25 4 2013 8 监测技术 5 1 2 1 ( 1. 江苏省疾病预防控制中心, 江苏南京 210009; 2. 南京医科大学第二附属医院, 江苏南京 210029) 5 Phenomenex kinetex C 18 2. 6 μm 4. 6 mm 150 mm 10 mmol /L ph 2. 5 + 60 40 DAD 280 nm 5 20. 0 mg /L ~ 100 mg /L 0. 02% 0. 03% 0. 02% 0. 04% 4 - - 2-0. 03% 82. 5% ~ 106% RSD 1. 4% ~ 6. 1% 82. 0% ~ 105% RSD 0. 4% ~ 2. 2% 78. 5% ~ 105% RSD 1. 7% ~ 4. 5% 4 - - 2 - O657. 7 + 2 B 1006-2009 2013 04-0031 - 05 Simultaneous Determination of Five Dyes in Hair Dying Formulations by Ion-Pair HPLC LI Li 1 XU Hai-e 2 JI Wen-liang 1 1. Jiangsu Center for Disease Control and Prevention Nanjing Jiangsu 210009 China 2. Nanjing Medical University Second Affiliated Hospital Nanjing Jiangsu 210029 China Abstract An ion-pair high performance liquid chromatographic method was established to simultaneous determination five dyes in oxidized hair dyes. The chromatographic conditions were as follows Phenomenex kinetex C 18 column 2. 6 μm 4. 6 mm 150 mm was selected with 10 mmol /L Octanesulfonic acid sodium solution ph 2. 5 -methanol 60 40 V /V as the mobile phase a diode array detector was used detection wavelength at 280 nm qualitative analysis by retention time and UV spectra characteristics quantitative analysis by external standard method. Results showed good linearity for the 5 compounds ranging from 20. 0 mg / L to 100 mg /L lowest detective limits for Quinhydrone is 0. 02% Resorcinol is 0. 03% o-aminophenol is 0. 02% o-phenylenediamine is 0. 04% 4-amino-2-hydroxytoluene is 0. 03%. Average spiked recoveries of matrices at lower level were between 82. 5% and 106% with RSD between 1. 4% and 6. 1%. Average spiked recoveries of matrices at middle level were between 82. 0% and 105% with RSD between 0. 4% and 2. 2%. Average spiked recoveries of matrices at high level were between 78. 5% and 105% with RSD between 1. 7% and 4. 5%. Key words Quinhydrone Resorcinol o-aminophenol o-phenylenediamine 4-amino-2-hydroxytoluene Ion-pair high performance liquid chromatographic Oxidized hair dyes ZX201109 2012-06 - 04 2013-04 - 18 1956 31
25 4. 5 2013 8 2. 20 g 1 000 ml 10% ph 2. 5 1. 2 色谱条件 2007 93 kinetex C 18 2. 6 μm 100 A 4. 6 mm 150 mm 25 5 μl A B 10 mmol /L 2 5-40 60 0. 25 ml /min 8 1. 3 样品前处理 1-2 + 0. 25 g 5 95 ph 7. 7 0. 000 1 g 25 ml 20 ml 8 25 20 min 3-4 4 1. 5 ml 1. 5 ml 9 13 000 r /min 5 min 0. 45 μm 5-8 1. 4 标准曲线绘制 5 0. 2 ml 0. 4 ml 0. 6 ml 0. 8 ml 1. 0 ml 10 6 8 20. 0 mg /L 4-40. 0 mg /L 60. 0 mg /L 80. 0 mg /L 100 mg /L - 2-2. 0% DAD 280 nm Phenomenex 3. 0% 5 μl 4 - - 2 - Rt 1 1. 1 主要仪器与试剂 2695 Waters 2996 AutoScience 20500A PHS - 3C ph Sartorius sigma 1-14 Mettler PM 200 2 2. 1 流动相的选择与优化 5 + 5 95 ph 7. 7 + 10 mmol /L 40 60 QK Dr. Ehrenstorfer. GmbH ph RCN 99% ph OAP 99% OPD 98% 2. 5 4 - - 2 - PAOC 97% Acros Organics 5 mmol /L ~ 5 1 000 mg /L 20 mmol /L 4 50. 0 mg 50 ml 30 ml 5 min 10 mmol /L 5 10 mmol /L 5 32
25 4. 5 2013 8 Rt 20. 05 min Rt 21. 53 min 4 - - 2 - Rt 35. 6 min 5 10 mmol /L 3 2. 2 色谱柱的选择 Zorbax SB - C 18 5 μm 4. 6 mm 250 mm Phenomenex kinetex C 18 5 1 2 3 10 Fig. 3 Chromatogram of 10 hair dyes 1 Zorbax SB - C 18 Fig. 1 Chromatogram of standard solution by Zorbax SB - C 18 column 4 Rt 21. 463 min 5 6 4-5 Fig. 4 4 Chromatogram of sample solution 2 Phenomenex kinetex C 18 Fig. 2 Chromatogram of standard solution by Phenomenex kinetex C 18 column 2. 3 干扰试验 PPD 2 5 - PTD PAP MAP PMAOS 5 Rt Fig. 5 UV spectrum of o-phenylenediamine 6. 76 min Rt 7. 83 min 33
25 4. 5 2013 8 2. 4 标准溶液稳定性试验 Fig. 6 5 4 24 h 24 h 5 48 h 20. 0 mg /L 72 h 15. 1% 60. 0 mg /L 6 6. 8% 20. 0 mg /L UV spectrum of impurities in the sample solution 1 Table 1 1 20. 0 mg /L Peak area change rate of mixed standard solution 20. 0 mg /L t /h 4 - - 2-0 410 246 343 293 270 338 392 375 341 888 24 416 841 342 611 267 356 377 695 340 737 48 431 779 356 324 258 673 372 450 333 062 72 435 309 353 013 229 470 370 492 325 754 [7-8] 2. 5 标准曲线与检出限 3 S /N = 3 5 20. 0 mg /L ~ 100 mg /L 3. 3 2 2 Table 2 2 The standard curve and the detection limit r m /μg m /μg y = 20 630x - 22 810 0. 999 9 0. 01 0. 04 0. 02 y = 17 516x - 5 633. 5 0. 999 9 0. 015 0. 05 0. 03 y = 12 461x + 35 275 0. 999 0 0. 01 0. 03 0. 02 y = 19 325x - 8 538. 2 0. 999 8 0. 02 0. 07 0. 04 4 - - 2 - y = 16 979x - 10 796 0. 999 9 0. 015 0. 05 0. 03 w /% 2. 6 精密度与加标回收试验 0. 6 ml 1. 0 ml 20. 0 mg /L 60. 0 mg /L 18 0. 25 g 100 mg /L 0. 000 1 g 6 1 1 000 mg /L 5 0. 2 ml 3 ρ / mg L - 1 3 n = 6 Table 3 Results of precision and spiked recovery test n = 6 ρ / mg L - 1 /% s / mg L - 1 RSD /% 20. 0 21. 3 106 0. 31 1. 5 60. 0 63. 1 105 0. 27 0. 4 100 105 105 1. 77 1. 7 20. 0 20. 3 102 0. 28 1. 4 60. 0 61. 5 102 0. 52 0. 8 100 103 103 1. 95 1. 9 20. 0 18. 3 91. 5 1. 11 6. 1 60. 0 49. 2 82. 0 1. 07 2. 2 34
25 4. 5 2013 8 ρ / mg L - 1 ρ / mg L - 1 /% s / mg L - 1 RSD /% 100 78. 5 78. 5 3. 50 4. 5 20. 0 16. 5 82. 5 0. 39 2. 4 60. 0 52. 6 87. 7 0. 69 1. 3 100 87. 8 87. 8 2. 60 3. 0 4 - - 2-20. 0 20. 3 102 0. 55 2. 7 60. 0 60. 2 100 0. 47 0. 8 100 102 102 2. 06 2. 0 2. 7 实际样品测定 4 4 7 4 < 10% 4 % Table 4 Determination results of samples % 4 - - 2-1 0. 58 0. 82 2 0. 82 0. 76 3 0. 43 0. 71 4 0. 59 0. 59 Fig. 7 3 7 The actual sample chromatogram 5 2006 16 7 7 2 2010 22 6 61-63. 4 - - 2-1. S. 2007. 2. M. 2003 135-405. 3. J. 2011 10 6 1-3. 4. 9 J. 2012 29 2 182-184. 5. - J. 2005 23 5 566. 6. J. 888-890.. - -3 J. 8. J. 2008 2 44-45. 檧檧檧檧檧 檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧檧 35