You Jingyan, Zhang Huarong, Zhang Hanqi, Yu Aimin, Xiao Tingting, Wang Yutang, Song Daqian
College of Chemistry, Jilin University, Changchun 130012, PR China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2007 Sep 1;856(1-2):278-84. doi: 10.1016/j.jchromb.2007.06.012. Epub 2007 Jun 22.
A method for determining triazine herbicides in infant nutrient cereal-based foods by pressurized microwave-assisted extraction (PMAE), coupled with high-performance liquid chromatography-electrospray ionization mass spectrometry (HPLC-ESI/MS), is described. The key parameters of PMAE, including extraction solvent, extraction time and temperature, were optimized. The isolation of the target compounds from the matrix was found to be efficient when 2 g of nutrient cereal samples was extracted with 20 mL of methanol for 10 min at 105 degrees C. Final determination was accomplished by HPLC-ESI/MS. The recoveries from 66.2 to 88.6% were obtained for three compounds at fortification levels (5-500 microg kg(-1)) with relative standard deviations (R.S.D.) <or=12.62%. Compared with atmospheric pressure microwave-assisted extraction (AMAE), ultrasonic extraction (UE) and soxhlet extraction (SE), the proposed method was more efficient, faster and more straightforward and required no additional cleanup steps. When the proposed method was applied to the aged spiked nutrient cereal samples, the results indicated that, although the recoveries of analytes were much lower than those obtained from fresh spiked samples, they were nevertheless satisfactory for the quantitative analysis of practical samples.
本文描述了一种通过加压微波辅助萃取(PMAE)结合高效液相色谱 - 电喷雾电离质谱(HPLC - ESI/MS)测定婴儿营养谷物类食品中三嗪类除草剂的方法。对PMAE的关键参数,包括萃取溶剂、萃取时间和温度进行了优化。当用20 mL甲醇在105℃下对2 g营养谷物样品萃取10 min时,发现从基质中分离目标化合物的效率很高。最终测定通过HPLC - ESI/MS完成。在加标水平(5 - 500 μg kg⁻¹)下,三种化合物的回收率为66.2%至88.6%,相对标准偏差(R.S.D.)≤12.62%。与常压微波辅助萃取(AMAE)、超声萃取(UE)和索氏萃取(SE)相比,该方法更高效、快速且直接,无需额外的净化步骤。当将该方法应用于老化的加标营养谷物样品时,结果表明,尽管分析物的回收率远低于新鲜加标样品,但对于实际样品的定量分析而言仍令人满意。