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目的建立分散固相萃取-高效液相色谱法测定水果中三氯生及三氯卡班残留的新方法。方法样品采用乙腈溶液涡旋超声提取后,加入十八烷基键合硅胶吸附剂(C18)作为分散固相萃取净化剂进行净化(200mg),用高效液相色谱法在278 nm处测定,采用PICKERING C8色谱柱(4.6 mm×250 mm i.d.,5μm),以甲醇:水(78:22,V:V)的溶液为流动相等度洗脱,流速1.2 m L/min。结果在最优检测条件下,各目标化合物的加标回收率为72.9%~104.4%,相对标准偏差在2.1%~9.1%之间。三氯生及三氯卡班的检出限分别为0.05和0.02 mg/kg,定量限分别为0.15和0.06 mg/kg。结论该方法分析快速、简便,适用于水果中三氯生及三氯卡班的测定。
OBJECTIVE To establish a new method for the determination of triclosan and triclocarbanin residues in fruits by dispersive solid-phase extraction-high performance liquid chromatography (HPLC). Methods The sample was extracted with acetonitrile by vortex and ultrasonic wave, then the octadecyl-bonded silica gel adsorbent (C18) was used as the dispersive solid-phase extraction scavenger to purify (200mg) and determined by high performance liquid chromatography at 278 nm. PICKERING C8 column (4.6 mm × 250 mm id, 5 μm) eluting with a mobile phase of methanol: water (78:22, V: V) at a flow rate of 1.2 mL / min. Results Under the optimum conditions, the spiked recoveries of the target compounds ranged from 72.9% to 104.4% with relative standard deviations between 2.1% and 9.1%. The detection limits of triclosan and triclocarban were 0.05 and 0.02 mg / kg, respectively. The limits of quantification were 0.15 and 0.06 mg / kg, respectively. Conclusion The method is rapid and simple and can be applied to the determination of triclosan and triclocarbanin in fruits.