目的建立基质分散固相萃取一高效液相测定板蓝根中药饮片中多茵灵残留的分析方法。方法样品经甲醇(含1%HAc,v/v)、氯化钠提取,用无水硫酸镁、PSA净化。使用cls柱(岛津VP-ODS150mmx4.6mm,5μm),流动相为甲:50mmol·L-1。Nall2P04(NaOH调节pH至6.O)=30:70,流速1.OmL‘min-1,检测波长284nm。结果该方法在0.0500-25.0mg·L-1范围内线性关系良好,检测限为0.01mg·L-1(s/N=3);在0.25—1.0rag·kgll范围内平均加样回收率为91.1%~103.3%(RSD〈2.5%)。采用该方法对市售板蓝根中药饮片中的多茵灵农药残留进行了检测。结论该方法快速简便、准确灵敏,能够满足板蓝根中药饮片中多茵灵农残的检测要求。
OBJECTIVE To establish an analytical method for determination of Carbendazim residue in Chinese decoction pieces of Isatis roots by dispersive solid phase extraction-HPLC. METHODS The samples were extracted by methanol (containing 1% HAc, v/v) and sodium chloride, and then were cleaned with anhydrous magnesium sul- fate and PSA. The detection was performed on a Cls column (Shimadzu VP-ODS 150mm x 4. 6mm ,5 ixm) with meth- anol:50mmol ~ L-1 and NaH2PO4 (adjusted to pH 6. 0 by NaOH) = 30:70 as the mobile phase, the flow rate was 1.0mL - min- 1, and the detection wavelength was 284nm. RESULTS The method had a good linear correlations at the concentration range of 0. 0500 to 25.0mg ~ L-1 and the detection limit of Carbendazim was 0. 0100mg ~ L-1 (S/ N =3). 1.0mg vailable The recoveries were in the range of 91.1% ~ 103.3% (RSD 〈 2. 5% ) at the concentration range of 0. 25 ~ ~ kg-1. This method was applied to the determination of Carbendazim pesticide residues in commercially a- Banlangen Herbal pieces. CONCLUSION This method is quick and easy, accurate and sensitive, and is a- ble to meet the requirements for determination of Carbendazim pesticide residues in Banlangen Herbal Pieces.