高效液相色谱法柱后衍生法测定陈皮中黄曲霉毒素

Determination of Aflatoxins in Citri Reticulatae Pericarpium by HPLC with Post-column Derivatization

目的考察医院药房中不同批次陈皮饮片中黄曲霉毒素B1,B2,G1,G2的含量,为确保陈皮饮片的临床用药安全。方法采用高效液相色谱法（HPLC）-碘柱后衍生化-荧光检测方法测定陈皮样品中黄曲霉毒素B1,B2,G1,G2的含量,色谱柱为Diamonsil C18柱（150 mm×4.6 mm,5μm）,流动相为甲醇-乙腈-水（40∶18∶42）,流速为0.8 m L/min,荧光检测,激发波长360 nm,发射波长450 nm。柱后碘衍生化系统为衍生溶液为0.05%的碘溶液,流速为0.3 m L/min,衍生化反应器温度为70℃。结果药房现存5批次陈皮样品均未检出黄曲霉毒素;黄曲霉毒素G2,G1,B1,B2进样量分别在1081 085 ng,2172 171 ng,1911 913 ng,64644 ng范围内与峰面积线性关系良好,加样回收率在60%110%之间。结论该方法准确、可靠,可作为陈皮中黄曲霉毒素的含量测定方法。

Objective To investigate the content of aflatoxin B_1,B_2,G_1,G_2 in different batches Citri Reticulatae Pericarpium,in order to ensure the safety of clinical use.Methods The content of aflatoxin B_1,B_2,G_1,G_2 was determined by HPLC with post- column derivatization.The chromatography was performed on a Diamonsil C_(18) column( 150 mm × 4.6 mm,5 um),with methanol- acetonitrile- water( 40 ∶ 18 ∶ 42) as the mobile phase,the flow rate was 0.8 m L / min; fluorescence detection,the excitation wavelength was 360 nm,the emission wavelength was 450 nm.The 0.05% iodine solution was used as the derivatization reagent,which was delivered at a flow rate of 0.3 m L / min and the reaction coil was maintained at 70℃.Results There were no aflatoxin was determined in the Citri Reticulatae Pericarpium.The linear range of aflatoxin G_2,G_1,B_1 and B_2 were 108- 1085 ng,217- 2171 ng,191- 1913 ng,64- 644 ng,respectively.The recover rate was 60%- 110%.Conclusion Aflatoxin was not detected in Citri Reticulatae Pericarpium which was safety and can be used for clinical prescription.The method is accurate and reliable,which can be used to control the content of aflatoxin in Citri Reticulatae Pericarpium.