高效液相色谱法测定椰油醇酰胺类表面活性剂中N-亚硝基二乙醇胺的含量
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摘要
采用高效液相色谱-紫外检测器测定椰油酸单乙醇酰胺和椰油酸二乙醇酰胺中的N-亚硝基二乙醇胺的含量。称取样品0.100 0g,用甲醇(8+2)溶液溶解并定容至10.0 mL,超声10min,经0.45μm微孔滤膜过滤后,滤液供高效液相色谱分析。以Diamonsil C_(18)硅胶键合相色谱柱(4.6mm×250mm,5μm)为固定相,以不同比例的甲醇-水体系为流动相进行梯度洗脱,采用紫外检测器在波长233nm处进行测定。N-亚硝基二乙醇胺的质量浓度在0.05～25.00mg·L~(-1)内与其峰面积呈线性关系,检出限(3S/N)和测定下限(10S/N)分别为15,48μg·L~(-1)。加标回收率在94.5%～98.5%之间,测定值的相对标准偏差(n=5)在3.8%～5.9%之间。
A method of high performance liquid chromatography-ultraviolet detector was applied to determination of N-nitrosodiethanolamine in coconut oil monoethanolamide and coconut oil diethanolamide.The sample(0.100 0 g) was dissolved in methanol(8+2) solution,and the solution was made up to 10.0 mL with methanol(8+2) solution.After ultrasonically extracting for 10 min,and filtering with 0.45μm micro filter membrane,the filtrate was analyzed by high performance liquid chromatography.Diamonsil C_(18) silica gel bonded phase column(4.6 mm×250 mm,5μm)was used as stationary phase,with a mixture of methanol and water with different ratios as mobile phase for gradient elution.UV detection was carried out at the wavelength of 233 nm.Linear relationship was found between chromatogaphic peak area and mass concentration of N-nitrosodiethanolamine in the range of 0.05-25.00 mg·L~(-1),with detection limit(3 S/N)and the lower limit of determination(10 S/N) of 15,48μg·L~(-1),respectively.Values of recovery obtained by standard addition method were in the range of 94.5%-98.5%,and relative standard deviations(n=5) were in the range of 3.8%-5.9%.
A method of high performance liquid chromatography-ultraviolet detector was applied to determination of N-nitrosodiethanolamine in coconut oil monoethanolamide and coconut oil diethanolamide.The sample(0.100 0 g) was dissolved in methanol(8+2) solution,and the solution was made up to 10.0 mL with methanol(8+2) solution.After ultrasonically extracting for 10 min,and filtering with 0.45μm micro filter membrane,the filtrate was analyzed by high performance liquid chromatography.Diamonsil C_(18) silica gel bonded phase column(4.6 mm×250 mm,5μm)was used as stationary phase,with a mixture of methanol and water with different ratios as mobile phase for gradient elution.UV detection was carried out at the wavelength of 233 nm.Linear relationship was found between chromatogaphic peak area and mass concentration of N-nitrosodiethanolamine in the range of 0.05-25.00 mg·L~(-1),with detection limit(3 S/N)and the lower limit of determination(10 S/N) of 15,48μg·L~(-1),respectively.Values of recovery obtained by standard addition method were in the range of 94.5%-98.5%,and relative standard deviations(n=5) were in the range of 3.8%-5.9%.
引文
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[4] FIUME M,HELDRETH B,BERGFELD W,et al.Safety assessment of ethanolamine and ethanolamine salts as used in cosmetics[J].International Journal of Toxicology,2015,34(2Suppl):84-98.
[5] QIAN Y,WU M,WANG W,et al.Determination of14nitrosamines at nanogram per liter levels in drinking water[J].Analytical Chemistry,2015,87(2):1330-1336.
[6] D′ISCHIA M,NAPOLITANO A,MANINI P,et al.Secondary targets of nitrite-derived reactive nitrogen species:Nitrosation/nitration pathways,antioxidant defense mechanisms and toxicological implications[J].Chemical Research in Toxicolog,2011,24(12):2071-2092.
[7] MEYER T A,POWELL J B.Quantitation of the nitrosamine 2-ethylhexyl-4-(N-methyl-N-nitrosoamino)benzoate(NPABAO)in sunscreen products[J].Journal-Association of Official Analytical Chemists,1991,74(5):766-771.
[8] 化妆品生产企业卫生规范(2007年版)[S].
[9] SCHEEREN M,SABIK H,GARIPY C,et al.Determination of N-nitrosamines in processed meats by liquid extraction combined with gas chromatographymethanol chemical ionisation/mass spectrometry[J].Food Additives and Contaminants Part A-Chemistry Analysis Control Exposure &Risk Assessment,2015,32(9):1436-1447.
[10] HUANG M,CHEN H,FU S,et al.Determination of volatile N-nitrosamines in meat products by microwave-assisted extraction coupled with dispersive micro solid-phase extraction and gas chromatographychemical ionisation mass spectrometry[J].Food Chemistry,2013,138(1):227-233.
[11] DONG H,GUO X,XIAN Y,et al.A salting outacetonitrile homogeneous extraction coupled with gas chromatography-mass spectrometry method for the simultaneous determination of thirteen N-nitrosamines in skin care cosmetics[J].Journal of Chromatography A,2015,1422:82-88.
[12] 李菊清,周孝瑞,黄丹勇.HPLC法测定除草剂二甲戊乐灵中亚硝胺[J].理化检验-化学分册,2001,37(4):145-146.
[13] CHISVERT A,BENEDJ L,PEIRM,et al.Determination of N-nitrosodiethanolamine in cosmetic products by reversed-phase dispersive liquid-liquid microextraction followed by liquid chromatography[J].Talanta,2017,166:81-86.
[14] SCHOTHORST R C,STEPHANY R W.Occurrence of N-nitrosodiethanolamine(NDELA)in cosmetics from the Dutch market[J].International Journal of Cosmetic Science,2001,23(2):109-114.
[15] 马强,王超,白桦,等.同位素稀释液相色谱-串联质谱法测定化妆品中的N-亚硝基二乙醇胺[J].色谱,2009(3):283-287.