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Determination of alkyltrimethylammonium chlorides in river water by gas chromatography/ion trap mass spectrometry with electron impact and chemical ionization

机译:电子轰击-化学电离气相色谱/离子阱质谱法测定河水中的烷基三甲基氯化铵

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This work describes a modified method to analyze alkyltrimethylammonium chlorides (ATMACs) in river water samples. The proposed method involves adding solid potassium iodide to water sample (pH adjusted to 10.0) as a counterion to enhance the extraction of ATMAC residues by dichloromethane liquid-liquid extraction. The iodide-ATMA(+) ion pairs were demethylated to their corresponding nonionic alkyldimethylamines (ADMAs) by thermal decomposition in a GC injection port. The corresponding ADMAs were then identified and quantitated by gas chromatography/ion trap mass spectrometry (GC/MS) in electron impact and low-pressure positive ion chemical ionization (PICI) modes. A relatively high abundance of ADMAs was detected at a demediylation temperature above 300 degreesC in the injection port. Experimental results indicate that the proposed method is precise and sensitive in ATMACs analysis and allows quantitation at less than or equal to 0.01 mug/L in 500 mL of the water samples. The enhanced selectivity of quasi-molecular ion chromatograms Of C-12-C-18-ADMA, obtained using methanol PICI-MS, enables ATMAC residues to be identified at trace levels in environmental samples. Recovery of the ATMACs in various spiked water samples ranged from 70 to 94% while RSD ranged from 3 to 12%. The concentrations of total measured ATMAC residues in river water samples ranged from nondetectable to 1.24 mug/L. [References: 45]
机译:这项工作描述了一种改进的方法来分析河水样品中的烷基三甲基氯化铵(ATMAC)。拟议的方法涉及向水样品中添加固体碘化钾(pH值调整为10.0)作为抗衡离子,以增强二氯甲烷液-液萃取对ATMAC残留物的萃取。通过在GC进样口中进行热分解,将碘化物-ATMA(+)离子对脱甲基成其相应的非离子烷基二甲基胺(ADMA)。然后通过气相色谱/离子阱质谱(GC / MS)在电子碰撞和低压正离子化学电离(PICI)模式下对相应的ADMA进行识别和定量。在注入口中高于300摄氏度的脱甲基温度下检测到相对较高的ADMA含量。实验结果表明,所提出的方法在ATMACs分析中是精确而灵敏的,并且可以在500 mL的水中进行小于或等于0.01 cup / L的定量。使用甲醇PICI-MS获得的C-12-C-18-ADMA准分子离子色谱图的更高的选择性使ATMAC残留物能够在环境样品中以痕量水平被鉴定出来。各种加标水样中ATMAC的回收率为70%至94%,而RSD为3%至12%。河水样品中测得的总ATMAC残留浓度范围为不可检测到1.24马克杯/升。 [参考:45]

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