基质分散固相萃取-高效液相色谱法测定板蓝根中药饮片中多菌灵的残留量  

Determination of carbendazim residue in Chinese decoction pieces of Isatis Roots by Dispersive Solid Phase Extraction-HPLC

作　　者：杨璐[1] 代琳男[1] 李丽[1] 陈菁[1] 江翠萍[1] 陈蓉[2,3] 

机构地区：[1]中国药科大学药学院,南京210009 [2]中国药科大学理学院分析化学教研室,南京2100091 [3]中国药科大学药品质量与安全预警教育部重点实验室,南京2100091

出　　处：《海峡药学》2013年第9期65-68,共4页Strait Pharmaceutical Journal

基　　金：江苏省省级大学生创新创业训练计划项目学生项目;国家基础科学人才培养基金(J0630858)

摘　　要：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.

关 键 词：多菌灵 板蓝根 基质分散固相萃取 高效液相色谱 

分 类 号：R282.71[医药卫生—中药学] R927.2[医药卫生—中医学]