纺织学报 ›› 2012, Vol. 33 ›› Issue (1): 96-101.

• 染整与化学品 • 上一篇    下一篇

基于超高效液相色谱-串联质谱法的纺织品中7种尼泊金酯类防腐剂测定

吴刚1,赵珊红1,吴俭俭1,董锁拽2,郭方龙1,王力君1,叶庆富3   

  1. 1. 浙江省检验检疫科学技术研究院
    2. 浙江大学原子核农业科学研究所
    3. 浙江出入境检验检疫局丝类检测中心
  • 收稿日期:2011-02-15 修回日期:2011-09-07 出版日期:2012-01-15 发布日期:2012-01-10
  • 通讯作者: 吴刚 E-mail:wg@ziq.gov.cn
  • 基金资助:

    国家级

Determination of 7 Nipagin Esters in Textiles by Ultra Performance Liquid Chromatography Coupled with Quadrupole Mass Spectrometry

  • Received:2011-02-15 Revised:2011-09-07 Online:2012-01-15 Published:2012-01-10
  • Contact: WU Gang E-mail:wg@ziq.gov.cn

摘要: 利用超高压液相色谱-电喷雾串联四极杆质谱(UPLC-MS/MS)联用技术,建立了一种能在7min内快速分离和测定纺织品中7种尼泊金酯类防腐剂的方法。样品经超声提取、浓缩,甲醇+水(1+1)溶解,采用ACQUITY UPLC?BEH C18柱(50 mm × 2.1 mm i.d.,1.7μm),以甲醇-水溶液为流动相,梯度洗脱,目标分析物采用UPLC-MS/MS进行分析,以保留时间和离子对进行定性和定量测定,在ESI(-)和MRM监测模式下进行样品分析。该方法检出限(LOD)为4~12μg/kg;在0.1~1.0μg/mL范围内线性关系良好,添加浓度分别为0.5mg/kg,1.0mg/kg和3.0mg/kg时,添加回收率范围为76.09 ± 4.92~106.65 ± 4.90%,相对标准偏差为4.60~14.01%。

Abstract: A novel method has been developed for the rapid separation and determination of 7 nipagin esters in textiles by ultra performance liquid chromatography-quadrupole mass spectrometry (UPLC-MS/MS) in 7 min. Nipagin esters residues in textiles were extracted by ultrasonic extraction with methanol. The extract was dried and redissolved in the mixed solvent of methanol and water (1+1). The chromatographic analysis was performed on an ACQUITY UPLC? BEH C18 column (50 mm × 2.1 mm i.d.,1.7μm ) by a gradient elution employing of methanol and water as a mobile phase. The analytes were detected using electrospray ionization (ESI) tandem mass spectrometry with multiple reaction monitoring (MRM) in negative ion mode. The calibration curves showed good linearity in the range of 0.1-1.0μg/mL for all nipagin esters with the limits of determination (LOD) of 4-12μg/kg. The recoveries of 7 nipagin esters at the spiked concentration levels of 0.5,1.0 and 3.0 mg/kg ranged from 76.09 ± 4.92 to 106.65 ± 4.90% with RSD of 4.60-14.01%.

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