骨折挫伤胶囊中黄曲霉毒素的测定

Determination of aflatoxin in Fracture Bruise Capsules

目的 用高效液相色谱柱后光化学衍生法对骨折挫伤胶囊中的黄曲霉毒素B_(1)、B_(2)、G_(1)、G_(2)进行含量测定。方法 用Persuit 5 C_(18)色谱柱(250 mm×4.6 mm,5μm);流动相为甲醇-乙腈-水(27∶12∶61)(A)-甲醇(B),梯度洗脱;流速为0.8 mL·min^(-1);激发波长λ_(ex)为360 nm,发射波长λ_(em)为450 nm;柱温为30℃。结果 黄曲霉毒素B_(1)、B_(2)、G_(1)、G_(2)分别在0.52~5.20、0.19~1.90、0.54~5.40、0.19~1.90 ng·mL^(-1)范围内线性关系良好;平均回收率分别为84.90%、85.32%、85.37%、81.92%。138批样品中有7批检出黄曲霉毒素B_(1)、G_(1),但均未超过限度,其余均未检出。结论 建立的方法可快速、简便、准确地检测骨折挫伤胶囊中黄曲霉毒素的含量,样品的测定结果也说明所测138批样品在黄曲霉毒素方面不存在安全性风险。

Objective To determine the content of aflatoxin B_(1),B_(2),G_(1) and G_(2) in Fracture Bruise Capsules by HPLC-photochemical derivatization.Methods The separation was achieved on a Persuit 5 C_(18) column(250 mm×4.6 mm,5 μm) at 30 ℃.The mobile phase consisted of methanol-acetonitrile-water(27∶12∶61)(A)-methanol(B) with gradient elution,and the flow rate was 0.8 mL·min^(-1).The excitation wavelength λ_(ex)=360 nm and the emission wavelength λ_(em)=450 nm.Results Aflatoxin B_(1),B_(2),G_(1) and G_(2)showed good linear relationships in the ranges of 0.52-5.20,0.19-1.90,0.54-5.40 and 0.19-1.90 ng·mL^(-1),and their average recoveries were 84.90%,85.32%,85.37% and 81.92%,respectively.Aflatoxin B_1 and G_1 were detected in 7 batch samples from 138 batches inspection,but all did not exceed the limit.The rest were not detected.Conclusion The established method can quickly,easily and accurately detect the content of aflatoxin in Fracture Bruise Capsules.The sample determination results also illustrate the measured 138 batch samples had no security risk in terms of aflatoxin.