建立了快速测定纺织助剂中双(氢化牛脂基)二甲基季铵化合物( DHTDMAC)的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。样品经5%(v/v)甲酸甲醇超声波提取、稀释后,采用Eclipse Plus C18柱(50 mm×2.1 mm,1.8μm)分离,甲醇和0.1%( v/v)甲酸水溶液为流动相梯度洗脱,电喷雾离子源正离子多反应监测模式进行定性和定量分析。实验结果表明,DHTDMAC在10~280μg/L范围内与峰面积呈良好的线性关系,相关系数( r2)为0.9991;以不低于3倍信噪比计算方法检出限( LOD,S/N=3)为3 mg/kg;方法定量限( LOQ,S/N=10)为10 mg/kg。3种纺织助剂基质中 DHTDMAC 在3个不同加标水平的平均回收率为97.2%~108.3%,相对标准偏差( RSD)为1.5%~4.6%。该方法灵敏度高、操作简便、快速准确,适用于纺织助剂中 DHTDMAC的分析测定。
A method has been developed for the determination of di( hydrogenated tallow alkyl)dimethyl ammonium compounds( DHTDMAC ) in textile auxiliaries by ultra-high per-formance liquid chromatography-tandem mass spectrometry ( UPLC-MS/MS ). The samples were extracted and diluted with acidified methanol by 5%( v/v)formic acid under ultrasonic assistance. The separation was performed on an Eclipse Plus C18 column( 50 mm × 2. 1 mm, 1. 8 μm)using 0. 1%( v/v)formic acid solution and methanol as the mobile phases. Identifica-tion and quantification were achieved by UPLC-MS/MS with electrospray ionization ( ESI ) source in positive ion mode and multiple reaction monitoring( MRM)mode. The results indica-ted that the calibration curve of DHTDMAC showed good linear relationship between peak area and mass concentration in the range of 10-280 μg/L with the correlation coefficient( r2)of 0. 999 1. The limit of detection( LOD,S/N=3)and the limit of quantification( LOQ,S/N=10) of this method were 3 mg/kg and 10 mg/kg,respectively. The average recoveries from three typical textile auxiliary matrices including dispersant,anti-static agent and fabric softener,at three spiked levels were in the range of 97. 2%-108. 3% with the relative standard deviations ( RSDs)of 1. 5%-4. 6%. The method is sensitive,accurate,simple and effective for the analysis of DHTDMAC in textile auxiliaries.
参考文献
[1] | Gerike P,Klotz H,Kooijman J G A,et al. Water Res,1994, 28(1):147,1994. |
[2] | Breen D,Horner J M,Bartle K D,et al. Water Res,1996, 30(2):476,1996. |
[3] | Institute for Health and Consumer Protection(IHCP). Euro-pean Union Risk Assessment Report:Dimethyldioctadecyl-ammonium Chloride.【2012-06-06】. http://echa.europa.eu/documents/10162/46f2f114-12ff-4af4-8da7-72148b6a202e,2012. |
[4] | European Chemicals Agency(ECHA). Quaternary Ammoni-um Compounds,Bis(hydrogenated tallow alkyl)dimethyl, chlorides.【2013-12-16】. http://apps.echa.europa.eu/regis-tered/data/dossiers/DISS-9ea9dcb9-7848-3271-e044-00144f-67d031/AGGR-fab45abb-836b-4a05-a42e-d0ec391c1cae DISS-9ea9dcb9-7848-3271-e044-00144f67d031. html # L-0b8f67c7-138a-421d-9947-f56bf4f435dd,2013. |
[5] | Levinson M I. J Surfact Deterg,1999,2(2):223,1999. |
[6] | Bernd W,Jurgen F. Rev Pro Color,2002,32(1):118,2002. |
[7] | Zhu F,Wei M,Yang Y R,et al. Journal of Chinese Mass Spectrometry Society(朱峰,卫敏,杨瑜榕,等. 质谱学报), 2014,35(6):563,2014. |
[8] | Comber S D W,Rule K L,Conrad A U,et al. Environ Pol-lut,2008,153(1):184,2008. |
[9] | García M T,Campos E,Sánchez-Leal J,et al. Chemo-sphere,2000,41(5):705,2000. |
[10] | Sun H F,Takata A,Hata N,et al. J Environ Monit,2003, 5(6):891,2003. |
[11] | 2002/371/EC,2002. |
[12] | The International Working Group on Global Organic Textile Standard. Global Organic Textile Standard(GOTS),2011,2011. |
[13] | Norwegian Pollution Control Authority. Draft of New Chap-ter Concerning Consumer Products in the Norwegian Prod-uct Regulations,2007,2007. |
[14] | Li X L,Brownawell B J. Environ Sci Technol,2010,44 (19):7561,2010. |
[15] | Martínez-Carballo E,Sitka A,Gonzáez-Barreiro C,et al. Environ Pollut,2007,146(2):543,2007. |
[16] | Li X L,Brownawell B J. Anal Chem,2009,81(19):7926,2009. |
[17] | Michael R,Thilo B,Jurgen F,et al. Anal Chem,1999,71 (23):5362,1999. |
[18] | Fernandez P,Alder A C,Suter M J F,et al. Anal Chem, 1996,68(5):921,1996. |
[19] | Martínez-Carballo E,Gonzáez-Barreiro C,Sitka A,et al. Environ Pollut,2007,145(2):489,2007. |
[20] | Voorde A,Lorgeoux C,Gromaire M C,et al. Environ Pol-lut,2012,164:150,2012. |
[21] | Nitschke L,Miiller R,Metzner G,et al. Fresenius J Anal Chem,1992,342(9):711,1992. |
[22] | Wee V T,Kennedy J M. Anal Chem,1982,54(9):1631,1982. |
[23] | Li Q Z,Zhou M H,Yue D L,et al. Journal of Instrumental Analysis(李全忠,周明辉,岳大磊,等. 分析测试学报), 2011,30(12):1444,2011. |
- 下载量()
- 访问量()
- 您的评分:
-
10%
-
20%
-
30%
-
40%
-
50%