分散液液微萃取-高效液相色谱串联质谱法快速测定水迁移相中甲醛

Rapid analysis of aqueous migration of formaldehyde by dispersive liquid-liquid micro-extraction and high performance liquid chromatography-tandem mass spectrometry

建立了分散液液微萃取-高效液相色谱串联质谱法快速测定轻纺消费品水迁移相中痕量甲醛的分析方法。水迁移相甲醛首先与2，4-二硝基苯肼（2，4-DNPH）衍生化反应生成甲醛-2，4-二硝基苯腙，优化的反应时间为15min，2，4-DNPH浓度为5mmol／L，HCl浓度为50mmol／L；在分散液液微萃取过程中，以500止乙腈为分散剂、50止四氯乙烯为萃取剂瞬间完成衍生物的萃取富集后，进行HPLC—ESI—MS／MS分析，分析时间为3．5min。水相中甲醛的检测线性范围为0．001～1mg／L，线性相关系数（R。）为0．9987，检出限为0．25斗∥L。平均加标回收率范围在82．8％～113．5％，相对标准偏差范围在2．1％～9．2％，平均富集倍数为120。方法已经应用于轻纺消费品水迁移相中甲醛含量的测定。

A new method of dispersive liquid-liquid micro-extraction （DLLME） and high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS） was established for the determination of trace formaldehyde in aqueous solution from light and textile consuming product. In the method, firstly, the aqueous formaldehyde was derivatized with 2, 4-dinitrophenylhydrazine （2,4-DNPH）, and then the derivative was extracted and enriched by DLLME using tetrachloroethylene as the extraction solvent and acetonitrile as disperser solvent. The experimental parameters affecting the derivatizing reaction and extraction recoveries of formaldehyde by DLLME were optimized. The results show that the linear range was 0. 001 - 1 mg/L, the linear correlation coefficient R2 was 0. 9987, the relative standard deviations were 2. 1% - 9. 2%, the average recoveries were 82. 8% - 113.5% , the method detection limit was 0. 25 μg/L, and the average enrichment factor was 120. The method was applied to determination of trace formaldehyde in aqueous solution from light and textile consuming products.