目的 建立超高效液相色譜-熒光法測定丹參飲片中黃曲霉毒素B₁、B₂、G₁、G₂。方法 樣品經(jīng)70%甲醇提取，通過免疫親和柱凈化后，用超高效液相色譜-熒光法進(jìn)行分析測定，WatersAcquity UPLC BEH C₁₈色譜柱（100 mm×2.1 mm，1.7 μm）；流動(dòng)相為甲醇-乙腈（1∶1）、水，梯度洗脫；體積流量0.4 mL/min；柱溫30℃；熒光檢測器激發(fā)波長365 nm；發(fā)射波長456 nm；進(jìn)樣量2 μL。結(jié)果 黃曲霉毒素B₁、B₂、G₁、G₂分別在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內(nèi)線性關(guān)系良好，r均大于0.99；定量限分別為0.10、0.03、0.39、0.03 ng/mL；黃曲霉毒素B₁的回收率為107%，RSD為6%；黃曲霉毒素總含量的回收率為80%，RSD為9%。專屬性、重復(fù)性、精密度、穩(wěn)定性試驗(yàn)均符合檢測要求。結(jié)論 所建立的方法準(zhǔn)確、可靠、專屬性強(qiáng)，可準(zhǔn)確地測定丹參飲片中黃曲霉毒素的含量。

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.

R284.1