大孔树脂提取西洋参总皂苷苯系残留限量检查

Limit Test of Benzene-series Residues in the Total-saponins of Separated and Purified by Macro Reticular Resin from Panax quinque folium L.

目的建立大孔树脂分离纯化西洋参总皂苷的苯系残留限量检查方法。方法采用项空-气相色谱法，色谱柱：HP-INNOWAX柱（60m×0．32mm，0．5μm）；检测器：FID；程序升温。结果线性范围（μg／mL）：苯1．2176～12．176，甲苯1．1749～11．749，二甲苯1．162～11．63，苯乙烯1．176～11．76，二乙烯基苯1．211～12．11；精密度（RSD％）：苯2．84，甲苯2．81，二甲苯2．90，苯乙烯2．62，二乙烯基苯2．69；最低检测限（μg／ml）：苯0．038，甲苯0．026，二甲苯0．049，苯乙烯0．028，二乙烯基苯0．099；三批样品均符合限量规定。结论采用本法检查大孔树脂分离纯化西洋参总皂苷的苯系残留限量方便、快速、准确，专属性好，并提示对同类分离纯化产品的苯系残留限量检查有指导意义。

Objective To establish a limit test of benzene-series residues in the total-saponins of separated and purified by macro reticular resin Panax quinque folium L.. Methods The following chromatographic tools were used to establish such a limit test, HS-GC with a flame-ionization detector, a HP-INNOWAX capillary column（60m × 0. 32mm, 0. 5μm）, and a temperature program was employed during the analyses. Results The linear range of each component was as followed： benzenelwas 2176-12. 176（μg · mL^-1 ）, toluenelwas 1749-11. 749（μg · mL^-1 ）, dimethylbenzene was 1. 162-11.63（μg · mL^-1 ）, styrenel was 176-11. 76（μg· mL^-1）, distyrenel was211-12.11（μg· mL^-1）. The precise of each component was also tested （RSD%）： benzene2.84, toluene2.81, dimethylbenzene2.90, styrene2.62, dityrene2. 69, respectively; and the detection limit of each component was listed as benzene 0. 038（μg · mL^-1 ）, toluene 0. 026（μg · mL^-1 ）, dimethylbenzene 0. 049 （μg · mL^-1 ）, styrene0. 028 （μg · mL^-1 ）, distyrene0. 099 （μg · mL^-1）, respectively. And the limit of three batches of samples coincided with the requirements. Conclusion This method was proved to be accurate and sensitive after validation. It is suggested to be suitable to the limit test of benzene-series residues in the same kind of substance separated and purified by macro reticular resin.