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目的:尝试利用液相色谱-串联质谱法对软胶囊中药用油辅料内黄曲霉毒素B_1含量进行测定。方法:以甲醇-0.1%甲酸水溶液为溶剂提取软胶囊中花生油所含黄曲霉毒素B_1,离心后取上清液过中性氧化铝固相萃取小柱净化,浓缩后进样测定,以甲醇-0.1%甲酸流动相梯度洗脱,流速为0.3 ml·min~(-1),柱温:30℃,进样量:25μl。采用电喷雾离子化四极杆串联质谱,多反应监测方式测定样品的浓度。结果:黄曲霉毒素B_1在0.098~1.960μg·L~(-1)范围内线性关系良好(r=0.999 5),检出限为0.05μg·L~(-1),平均加样回收率为97.73%,RSD=4.625%(n=6)。结论:此法灵敏准确,专属性强,干扰少,重现性佳,对含油药物制剂中黄曲霉毒素B_1含量检测有参考意义。
OBJECTIVE: To determine the content of aflatoxin B 1 in traditional Chinese medicine oil excipients by using liquid chromatography-tandem mass spectrometry. Methods: The aflatoxin B_1 in peanut oil was extracted with methanol - 0.1% formic acid as the solvent. The supernatant was centrifuged and neutralized with neutral alumina solid phase extraction cartridge. After concentration, 0.1% formic acid gradient elution, flow rate of 0.3 ml · min -1, column temperature: 30 ℃, injection volume: 25μl. Electrospray ionization quadrupole tandem mass spectrometry was used to determine the concentration of the sample. Results: The linear range of aflatoxin B_1 was 0.098-1.960 μg · L -1 (r = 0.999 5). The detection limit was 0.05 μg · L -1. The average recovery was 97.73%, RSD = 4.625% (n = 6). Conclusion: The method is sensitive, accurate, specific, less perturbed and reproducible. It has reference value for the determination of aflatoxin B1 in oily drug preparations.