论文部分内容阅读
目的:建立HPLC-柱后光化学衍生法测定舒筋活血丸中黄曲霉毒素G2、G1、B2、B1的含量,并通过对72批样品检测结果的分析初步考察舒筋活血丸制剂在黄曲霉毒素污染方面的安全性,以提示企业选择合格安全的原料药材投料。方法:采用Diamonsil C18(4.6 mm×250 mm,5μm)色谱柱,以乙腈-甲醇-水为梯度洗脱流动相,流速1.1 mL·min-1,柱温40℃;采用柱后光化学衍生法,荧光检测器激发波长λex=360 nm、发射波长λem=450 nm。结果:黄曲霉毒素G2、G1、B2、B1分别在2.806~16.825 pg(r=0.9973)、9.830~58.983 pg(r=0.9998)、2.891~17.345 pg(r=0.9956)、9.9~59.4 pg(r=0.9966)范围内线性关系良好;黄曲霉毒素B1及总量回收率(n=6)分别为78.5%(RSD=1.6%)和85.5%(RSD=4.0%)。有27批样品检出黄曲霉毒素,其总量含量为0.007×10-3~39.87×10-3μg·g-1。结论:该方法经方法学验证可用于舒筋活血丸中黄曲霉毒素检测;建议增订舒筋活血丸中黄曲霉毒素检查项;建议企业重视动物类药材的质量和安全性。
OBJECTIVE: To establish an HPLC-column photochemical derivatization method for the determination of aflatoxins G2, G1, B2, B1 in Shujinhuoxue Pills. Through the analysis of 72 batches of samples, the effects of Shujinhuoxue Pill preparations on aflatoxins Pollution safety, to prompt businesses to choose qualified raw materials safe feed. METHODS: Diamonsil C18 (4.6 mm × 250 mm, 5 μm) was used as the mobile phase. The mobile phase was eluted with acetonitrile-methanol-water at a flow rate of 1.1 mL · min-1 and the column temperature was 40 ℃. Fluorescence detector excitation wavelength λex = 360 nm, emission wavelength λem = 450 nm. Results: Aflatoxins G2, G1, B2, and B1 were in the range of 2.806-16.825 pg (r = 0.9973), 9.830-58.983 pg (r = 0.9998), 2.891-17.345 pg = 0.9966); aflatoxin B1 and total recovery (n = 6) were 78.5% (RSD = 1.6%) and 85.5% (RSD = 4.0%), respectively. 27 batches of samples were detected aflatoxin, the total amount of 0.007 × 10-3 ~ 39.87 × 10-3μg · g-1. Conclusion: This method is validated by methodology and can be used to detect aflatoxins in Shujinhuoxue Pill. It is suggested that aflatoxin check items should be added in Shujinhuoxue Pill. Enterprises should pay attention to the quality and safety of animal medicines.