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

Determination of triclosan and triclocarban in fruit by dispersive solid-phase extraction and high performance liquid chromatography

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 develop a method for determination of triclosan and triclocarban in fruit by dispersive solid-phase extraction(DSPE) combined with high performance liquid chromatography(HPLC). Methods The analytes were supersonic extracted from the fruit samples by acetonitrile, and purified by dispersion solid phase extraction using C18 sorbent(200 mg), then analyzed by high performance liquid chromatography with 278 nm detector. The chromatographic separation was performed on a PICKERING C8column(4.6 mm×250 mm i.d., 5 μm), using a gradient elution program of methanol-H2O(78:22=V:V) as a mobile phase with a flow rate at 1.2 m L/min and the detector setting at 278 nm. Results Under optimization condition, the recoveries were in the range of 72.9%~104.4%, and the relative standard deviations(RSD) were 2.1%~9.1%. The limit of detection was 0.05 and 0.02 mg/kg, and the limit of quantification was 0.15 and 0.06 mg/kg for triclosan and triclocarban. Conclusion This method was quick and easy, and applicable to determination of triclosan and triclocarban in fruit.