g ml 10% ph 色谱条件 kinetex C μm 100 A 4. 6 mm 150 mm 25 5 μl A B 10 mmol /L ml /min

Size: px

Start display at page:

Download "g ml 10% ph 色谱条件 kinetex C μm 100 A 4. 6 mm 150 mm 25 5 μl A B 10 mmol /L ml /min"

玖江
6 years ago
Views:

1 监测技术 ( 1. 江苏省疾病预防控制中心, 江苏南京 ; 2. 南京医科大学第二附属医院, 江苏南京 ) 5 Phenomenex kinetex C μm 4. 6 mm 150 mm 10 mmol /L ph DAD 280 nm mg /L ~ 100 mg /L 0. 02% 0. 03% 0. 02% 0. 04% % 82. 5% ~ 106% RSD 1. 4% ~ 6. 1% 82. 0% ~ 105% RSD 0. 4% ~ 2. 2% 78. 5% ~ 105% RSD 1. 7% ~ 4. 5% O B 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 China 2. Nanjing Medical University Second Affiliated Hospital Nanjing Jiangsu 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 methanol 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 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 ZX

2 g ml 10% ph 色谱条件 kinetex C μm 100 A 4. 6 mm 150 mm 25 5 μl A B 10 mmol /L ml /min 样品前处理 g 5 95 ph g 25 ml 20 ml min ml 1. 5 ml r /min 5 min μm 标准曲线绘制 ml 0. 4 ml 0. 6 ml 0. 8 ml 1. 0 ml mg /L mg /L mg /L mg /L 100 mg /L % DAD 280 nm Phenomenex 3. 0% 5 μl Rt 主要仪器与试剂 2695 Waters 2996 AutoScience 20500A PHS - 3C ph Sartorius sigma 1-14 Mettler PM 流动相的选择与优化 ph mmol /L QK Dr. Ehrenstorfer. GmbH ph RCN 99% ph OAP 99% OPD 98% PAOC 97% Acros Organics 5 mmol /L ~ mg /L 20 mmol /L mg 50 ml 30 ml 5 min 10 mmol /L 5 10 mmol /L 5 32

3 Rt min Rt min Rt min 5 10 mmol /L 色谱柱的选择 Zorbax SB - C 18 5 μm 4. 6 mm 250 mm Phenomenex kinetex C 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 min 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 PTD PAP MAP PMAOS 5 Rt Fig. 5 UV spectrum of o-phenylenediamine min Rt min 33

4 标准溶液稳定性试验 Fig h 24 h 5 48 h mg /L 72 h 15. 1% mg /L % mg /L UV spectrum of impurities in the sample solution 1 Table mg /L Peak area change rate of mixed standard solution mg /L t /h [7-8] 2. 5 标准曲线与检出限 3 S /N = mg /L ~ 100 mg /L Table 2 2 The standard curve and the detection limit r m /μg m /μg y = x y = x y = x y = x y = x w /% 2. 6 精密度与加标回收试验 0. 6 ml 1. 0 ml mg /L mg /L g 100 mg /L g mg /L ml 3 ρ / mg L n = 6 Table 3 Results of precision and spiked recovery test n = 6 ρ / mg L - 1 /% s / mg L - 1 RSD /%

5 ρ / mg L - 1 ρ / mg L - 1 /% s / mg L - 1 RSD /% 实际样品测定 < 10% 4 % Table 4 Determination results of samples % Fig The actual sample chromatogram S M J J J J J. 8. J 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

中草药 Chinese Traditional and Herbal Drugs 第 5 卷第 1 期 201 年 1 月 51 其他试剂均为分析纯对照品栀子苷 ( 批号 1109-201115) 甘草苷 ( 批号 1110-201106) 连翘酯苷

中草药 Chinese Traditional and Herbal Drugs 第 5 卷第 1 期 201 年 1 月 51 其他试剂均为分析纯对照品栀子苷 ( 批号 1109-201115) 甘草苷 ( 批号 1110-201106) 连翘酯苷 50 中草药 Chinese Traditional and Herbal Drugs 第 5 卷第 1 期 201 年 1 月凉膈散汤剂 HPLC-DAD 指纹图谱研究 * 胡建兰, 邵萌, 余林中南方医科大学中医药学院, 广东广州 510515 摘要 : 目的研究凉膈散汤剂 HPLC-DAD 指纹图谱, 建