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目的:采用HPLC-MS/MS法测定巴天酸模中7个蒽醌类成分的含量。方法:采用SB-C_(18)色谱柱(4.6 mm×100 mm,1.8μm),流动相为乙腈(A)-0.1%甲酸水(B)。梯度洗脱程序为:0~8.5 min,95%~95%A;8.5~8.51 min,95%~40%A;8.51~12 min,40%~40%A。流动相流速为0.4 mL/min,柱温为20℃,进样量为10μL。结果:大黄酸、芦荟大黄素在2.5~50 ng/mL,大黄素、大黄素甲醚在10~250 ng/mL,大黄酚在25~1000 ng/mL,大黄素-8-O-葡萄糖苷、大黄素甲醚-8-O-葡萄糖苷在10~500 ng/mL范围内,进样量与峰面积具有良好线性关系(r~2均>0.98)。同时,其平均加样回收率在90.32%~106.75%(n=6)。结论:该方法简便、准确、灵敏,可用于巴天酸模中蒽醌类成分的含量测定。
OBJECTIVE: To determine the content of seven anthraquinones in P. acid by HPLC-MS / MS. Methods: The mobile phase consisted of acetonitrile (A) -0.1% formic acid (B) with SB-C18 column (4.6 mm × 100 mm, 1.8 μm). Gradient elution program: 0 ~ 8.5 min, 95% ~ 95% A; 8.5 ~ 8.51 min, 95% ~ 40% A; 8.51 ~ 12 min, 40% ~ 40% The mobile phase flow rate was 0.4 mL / min, the column temperature was 20 ℃ and the injection volume was 10 μL. Results: Rhein, aloe-emodin showed good performance in the range of 2.5-50 ng / mL, with emodin, physcion at 10-250 ng / mL, chrysophanol at 25-1000 ng / mL, emodin- There was a good linear relationship between the injection volume and the peak area (r ~ 2> 0.98) for the range of 10 ~ 500 ng / mL. At the same time, the average recovery rates ranged from 90.32% to 106.75% (n = 6). Conclusion: The method is simple, accurate and sensitive and can be used for the determination of anthraquinones in P. acidophilus.