Mesh : Tandem Mass Spectrometry / methods Vegetables / chemistry Fruit / chemistry Chromatography, High Pressure Liquid / methods Pesticide Residues / analysis Food Contamination / analysis Reproducibility of Results Limit of Detection

来  源:   DOI:10.1371/journal.pone.0307669   PDF(Pubmed)

Abstract:
A modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) -LC-MS/MS method was developed for the determination of hexachlorophene in fruits and vegetables. Samples were extracted by acetonitrile and then salted with an acetate buffer system. Extractants neutral alumina (Al-N), strong cation exchange silica gel bonded adsorbent (SCX) and graphitized carbon black (GCB) were used for sample purification. The method demonstrates excellent accuracy and reproducibility. Under optimized conditions, the correlation coefficients of hexachlorophene were higher than 0.995 in the range of 0.5-20 ng/mL. The limit of quantification (LOQ) was 2.0 μg/kg. The average recoveries, assessed at three spiked levels (2.0, 4.0, and 20.0μg/kg) across various matrices including cabbage, celery, tomato, eggplant, potato, radish, cowpea, chives, apple, peach, grape, citrus, bitter melon, banana and hami melon ranged from 72.0 to 100.5% with relative standard deviations from 3.2 to 9.8% (n = 6).
摘要:
修改后的QuEChERS(快速,Easy,便宜,有效,坚固而安全)-建立了测定水果和蔬菜中六氯苯的LC-MS/MS方法。样品用乙腈提取,然后用乙酸盐缓冲体系盐化。萃取剂中性氧化铝(Al-N),使用强阳离子交换硅胶键合吸附剂(SCX)和石墨化炭黑(GCB)进行样品纯化。该方法具有良好的准确性和重现性。在优化条件下,六氯酚在0.5-20ng/mL范围内的相关系数高于0.995。定量限(LOQ)为2.0μg/kg。平均回收率,在包括卷心菜在内的各种基质中以三个加标水平(2.0、4.0和20.0μg/kg)进行评估,芹菜,番茄,茄子,马铃薯,萝卜,牛仔,细香葱,苹果,桃子,葡萄,柑橘,苦瓜,香蕉和哈密瓜的相对标准偏差为3.2至9.8%(n=6),范围为72.0至100.5%。
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