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气相色谱-质谱联用同时测定水和土壤中的二苯甲酮类紫外线过滤剂

Simultaneous determination of benzophenone-type UV filters in water and soil by gas chromatography-mass spectrometry.

作者信息

Jeon Hee-Kyung, Chung Yong, Ryu Jae-Chun

机构信息

Toxicology Laboratory, Bioanalysis and Biotransformation Research Center, Korea Institute of Science & Technology P.O. Box 131, Chengryang, Seoul 130-650, South Korea.

出版信息

J Chromatogr A. 2006 Oct 27;1131(1-2):192-202. doi: 10.1016/j.chroma.2006.07.036. Epub 2006 Aug 7.

Abstract

A novel method has been developed to simultaneously determine and quantify seven organic UV filters employing liquid (solid)-liquid extraction, derivatization with N-methyl-N-(trimethylsilyl) trifluoroacetamide (MSTFA) and gas chromatography with mass spectrometric detection in various environmental matrices. The UV filters determined were: benzophenone (BP), benzhydrol (BH), 4-hydroxybenzophenone (HBP), 2-hydroxy-4-methoxybenzophenone (HMB), 2,4-dihydroxybenzophenone (DHB), 2,2'-dihydroxy-4-methoxybenzophenone (DHMB) and 2,3,4-trihydroxylbenzophenone (THB). Under optimal conditions, the analysis required 23 min and good linearity over the range of 10-2,500 ng/L in water and 100-25,000 ng/kg in soil for each UV filter obtained. The high recovery (62-114% and 60-125% for water and soil samples, respectively) and the low RSD values (less than 13.9 and 17.2% for water and soil samples, respectively) indicated the high performance of this method. The method detection limits (MDLs) were relatively low, ranging from 5 to 100 ng/L or kg and quantification limits ranged between 25 and 500 ng/L or kg for all test compounds. This validated method was applied in the analysis of seven BP-type UV filters collecting water and soil samples in Korea, between April and May 2003. The overall concentration of UV filters in the soil sample (500-18,380 ng/kg) was highly distributed in water sample (27-204 ng/L). The established method was successfully applied to monitor the residue measurement of the BP-type UV filters in environmental water and soil samples.

摘要

已开发出一种新方法,用于同时测定和定量七种有机紫外线过滤剂,该方法采用液(固)-液萃取、用N-甲基-N-(三甲基硅基)三氟乙酰胺(MSTFA)进行衍生化反应以及在各种环境基质中使用气相色谱-质谱检测法。所测定的紫外线过滤剂有:二苯甲酮(BP)、二苯甲醇(BH)、4-羟基二苯甲酮(HBP)、2-羟基-4-甲氧基二苯甲酮(HMB)、2,4-二羟基二苯甲酮(DHB)、2,2'-二羟基-4-甲氧基二苯甲酮(DHMB)和2,3,4-三羟基二苯甲酮(THB)。在最佳条件下,每次分析需时23分钟,且在水中浓度范围为10 - 2500 ng/L以及在土壤中浓度范围为100 - 25000 ng/kg时,每种紫外线过滤剂均具有良好的线性关系。高回收率(水样和土壤样分别为62 - 114%和60 - 125%)以及低相对标准偏差值(水样和土壤样分别小于13.9%和17.2%)表明该方法性能良好。方法检出限相对较低,所有测试化合物的检出限在5至100 ng/L或kg之间,定量限在25至500 ng/L或kg之间。该经过验证的方法应用于分析2003年4月至5月期间在韩国采集的水样和土壤样中的七种BP型紫外线过滤剂。土壤样中紫外线过滤剂的总浓度(500 - 18380 ng/kg)在水样(27 - 204 ng/L)中分布较高。所建立的方法成功应用于监测环境水样和土壤样中BP型紫外线过滤剂的残留量测定。

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