RESUMO
Objective:To establish a method for the determination of aflatoxin( AF) B1,B2,G1and G2by HPLC in Xiao'er Fupi granule,and help manufacturers select safe raw materials for production through the analysis of test results of 31 batches of samples and the safety investigation of Xiao'er Fupi granule in terms of aflatoxin pollution. Methods: A post-column photochemical derivation HPLC method was used to detect the content of aflatoxin in Xiao'er Fupi granule. An Ecosil C18column(250 mm×4.6 mm,5 μm) was adopted with the mobile phase of acetonitrile-methanol-water (30: 10: 60)at the flow rate of 0.8 ml·min-1. The column tem-perature was maintained at 30 ℃. The sample size was 20 μl,The excitation wavelength was 360 nm and the emission wavelength was 450 nm in the fluorescence detection. Results:The linear range of aflatoxin B1,B2, G1and G2was 9.65-48.25 pg (r=0.999 1), 2.45-12.25 pg(r=0.999 8), 10.5-52.5 pg(r =0.995 6) and 2.55-12.75 pg (r =0.996 6), respectively. The recovery was 83.3%-95.6%. Totally 14 batches of samples contained aflatoxin,and the total content was 0.21 × 10 -3-0.54 ×10 -3μg·g-1. Conclusion:The method is convenient and accurate,which can be used for the quality control of Xiao'er Fupi granule.
RESUMO
Objective:To determine aflatoxin B1 , B2 , G1 and G2 in Shugan pills by HPLC and evaluate their safety. Methods:The product was analyzed by HPLC using a Shiseido C18 column(150 mm × 4. 6 mm,5 μm)with methanol-acetonitrile-water (10 :30 :60) as the mobile phase. An ultraviolet lamp was derivative at 254 nm, and the fluorescence detection was performed with the excitation wavelength at 360 nm and the emission wavelength at 450nm. The samples from nation-wide market were detected by the method. Re-sults:Good linear relationships were obtained within the range of 10-50 pg for aflatoxin B1 and G1 , and 3-15 pg for aflatoxin B2 and G2 . The recovery of aflatoxin B1 , B2 , G1 and G2 was 89. 9%,87. 9%,86. 1% and 87. 1%,respectively with all the RSD below 3. 0%. The results of all samples were satisfactory, and the qualification rate of the samples was 100%, indicating that the samples were safe. Conclusion:The developed method is convenient and accurate, which can be applied in the quantitative determination of Shugan pills.
RESUMO
Objective:To determine aflatoxin B1 , B2 , G1 and G2 in Shugan pills by HPLC and evaluate their safety. Methods:The product was analyzed by HPLC using a Shiseido C18 column(150 mm × 4. 6 mm,5 μm)with methanol-acetonitrile-water (10 :30 :60) as the mobile phase. An ultraviolet lamp was derivative at 254 nm, and the fluorescence detection was performed with the excitation wavelength at 360 nm and the emission wavelength at 450nm. The samples from nation-wide market were detected by the method. Re-sults:Good linear relationships were obtained within the range of 10-50 pg for aflatoxin B1 and G1 , and 3-15 pg for aflatoxin B2 and G2 . The recovery of aflatoxin B1 , B2 , G1 and G2 was 89. 9%,87. 9%,86. 1% and 87. 1%,respectively with all the RSD below 3. 0%. The results of all samples were satisfactory, and the qualification rate of the samples was 100%, indicating that the samples were safe. Conclusion:The developed method is convenient and accurate, which can be applied in the quantitative determination of Shugan pills.