超高速液体クロマトグラフィー-タンデム質量分析法による繊維補助剤中のジ（水添タロウアルキル）ジメチルアンモニウム化合物の定量

[Determination of di (hydrogenated tallow alkyl) dimethyl ammonium compounds in textile auxiliaries by ultra-high performance liquid chromatography-tandem mass spectrometry].

• Feng Zhu

抄録

繊維助剤中のジ（水添タロウアルキル）ジメチルアンモニウム化合物（ＤＨＴＤＭＡＣ）を超高性能液体クロマトグラフィー-タンデム質量分析法で定量する方法が開発された。UPLC-MS/MS）を用いた。サンプルを超音波補助下で５％（ｖ／ｖ）ギ酸で酸性化メタノールで抽出し、希釈した。0.1%(v/v)ギ酸溶液とメタノールを移動相として使用し、Eclipse Plus C18カラム(50mm x 2.1mm, 1.8μm)上で分離を行った。正イオンモードおよび多重反応モニタリング（MRM）モードのエレクトロスプレーイオン化（ESI）源を用いたUPLC-MS/MSにより、同定および定量を行った。その結果、DHTDMACの検量線は10-280μg/Lの範囲でピーク面積と質量濃度の間に良好な直線関係を示し、相関係数(r2)は0.9991であった。本法の検出限界（LOD、S/N=3）は3 mg/kg、定量限界（LOQ、S/N=10）は10 mg/kgであった。分散剤、帯電防止剤、柔軟剤を含む3つの典型的な繊維補助マトリックスからの平均回収率は97.2%～108.3%の範囲であり、相対標準偏差（RSD）は1.5%～4.6%であった。この方法は、繊維助剤中のDHTDMACの分析に感度が高く、正確で、簡単で、効果的である。

A method has been developed for the determination of di (hydrogenated tallow alkyl) dimethyl ammonium compounds (DHTDMAC) in textile auxiliaries by ultra-high performance 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 x 2.1 mm, 1.8 microm) using 0.1% (v/v) formic acid solution and methanol as the mobile phases. Identification 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 indicated that the calibration curve of DHTDMAC showed good linear relationship between peak area and mass concentration in the range of 10-280 microg/L with the correlation coefficient (r2) of 0.9991. 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, antistatic 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.