[关键词]
[摘要]
目的 建立超高效液相色谱-荧光法测定丹参饮片中黄曲霉毒素B1、B2、G1、G2。方法 样品经70%甲醇提取,通过免疫亲和柱净化后,用超高效液相色谱-荧光法进行分析测定,WatersAcquity UPLC BEH C18色谱柱(100 mm×2.1 mm,1.7 μm);流动相为甲醇-乙腈(1∶1)、水,梯度洗脱;体积流量0.4 mL/min;柱温30℃;荧光检测器激发波长365 nm;发射波长456 nm;进样量2 μL。结果 黄曲霉毒素B1、B2、G1、G2分别在0.120 1~1.920 8、0.036 1~0.577 2、0.122 1~1.954 0、0.042 1~0.673 2 ng/mL内线性关系良好,r均大于0.99;定量限分别为0.10、0.03、0.39、0.03 ng/mL;黄曲霉毒素B1的回收率为107%,RSD为6%;黄曲霉毒素总含量的回收率为80%,RSD为9%。专属性、重复性、精密度、稳定性试验均符合检测要求。结论 所建立的方法准确、可靠、专属性强,可准确地测定丹参饮片中黄曲霉毒素的含量。
[Key word]
[Abstract]
Objective To establish an ultra performance liquid chromatography-fluorescence detection method for determination of aflatoxin B1,B2,G1,G2 in Salvia miltiorrhiza pieces. Methods After being extracted by 70% methanol solution and purification by immune affinity columns, aflatoxin B1,B2,G1,G2 were analyzed by ultra performance liquid chromatography-fluorescence detection. Chromatographic conditions were as follows:Acquity UPLC BEH C18 column (100 mm×2.1 mm, 1.7 μm), the mobile phase consisted of methanol-acetonitrile (1:1) and water with gradient elution, volume flow was 0.4 mL/min, column temperature was 30℃, excitation wavelength of fluorescence detector was 365 nm; the emission wavelength was 456 nm; injection volume was 2 μL. Results Aflatoxin B1 showed a good linear relationship at a range of 0.120 1-1.920 8 ng/mL, a-flatoxin B2at a range of 0.036 1-0.577 2 ng/mL, aflatoxin G1 at a range of 0.122 1-1.954 0 ng/mL and aflatoxin G2 at a range of 0.042 1-0.673 2 ng/mL, r ≥ 0.99. The quantitation limits are 0.10, 0.03, 0.39, 0.03 ng/mL. The recovery of aflato-xin B1 was 107% and RSD was 6%. The recovery of total aflatoxin content was 80% and RSD was 9%. The specificity, repeatability, precision and stability tests all meet the testing requirements. Conclusion The established method is accurate, reliable and specific, it can accurately determine the content of aflatoxin in Salvia miltiorrhiza pieces.
[中图分类号]
R284.1
[基金项目]