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Determination of aflatoxin B1 in Chinese herbal medicine content


Tested by mixing crushed herbs, weighed 5.00g, release 100ml conical flask with stopper, the addition of 40ml of methanol water (55:45), ultrasound 20min, and then filtration and washing dregs and the filter, the filtrate was 150m1 separating funnel with 20ml, 15ml chloroform extraction twice, chloroform layer through a funnel filled with anhydrous sodium sulfate, filter one pan in water bath at 65c 【= play dry, cool one with 1ml of benzene acetonitrile (98:2) at constant volume, microporous membrane (0.45m) filter and set aside. 2.4 Standard Curve take 0.1mg/ml standard solution,[link widoczny dla zalogowanych], absorb 0.5mL, 1.0mL, 1.5mL, 2.0mL, 2.5mL, 10mL volumetric flask in the home, plus a benzene acetonitrile (98 : 2) diluted to the mark, shake, absorb 20L (20L loop) injection of high performance liquid chromatography, the sample volume to the reference solution for the abscissa and peak area value of y is the vertical axis, the standard curve, the results show: aflatoxin B in the range of 0.05 ~ 0.66tLg peak area was linear regression equation was: Y = 0.47869 +8.71639, r = 0.99993. 2.5 Precision draw the same concentration of test precision of aflatoxins B, the reference solution 20L, injection high performance liquid chromatography, repeated sampling 5 times, peak area determination, the result: RSD 1.5%. 2.6 repeatability and stability test repeated measurements on the same batch of samples 5, RSD 2.2%. Repeated measurements within the 2h, from RSD = 2.3%. The repeatability and stability are good. Known content of 2.7 to take recovery test samples Zushima 2.00g, respectively,[link widoczny dla zalogowanych], added precision of aflatoxin B, reference substance, after preparation and extraction by 2.3, take 20L injection content was determined by high performance liquid chromatography, the results Table 1. Table 1 Number of aflatoxin B content of the sample recovery test adding amount (g) (g) measured value (g) the average recovery rate (%)(%) RSD (%) 94.4050.0050.0010o. 0o100.00150.00150.00141.05143.75190.40190.70237.95235.5593.3098.7096.0095.681.9796.3095.7094.1012345636 Yong: Determination of aflatoxins in traditional Chinese medicine B, determination of the content of the sample, accurately weighed 2.8 8 medicines each 5.00g, prepared by extracting 2.3, the check 201. LL content was determined by high performance liquid chromatography to determine the results in Table 2. Chromatogram shown in Figure 1, Figure 2. Figure 1 Standard AF-B. Figure 2 Zushima medicine AF-B samples of 28 kinds of Chinese herbal medicines in the form of aflatoxin B, content of the sample content sample content (g / kg) (g / kg) of gold fruit Lan Shegan not detected not detected Zushima 724.5 Thin leather is not detected not detected in almonds Codonopsis Astragalus 113.6 33.9 3 big Fu to discuss the skin was not detected in the detection of eight herbs 3.1, the founder of Ma, astragalus, almond content of aflatoxin B1 is: 724.5wg/kg,[link widoczny dla zalogowanych], 113.6g/kg,[link widoczny dla zalogowanych], 33.9g/kg, the remaining five were not detected from the outside of aflatoxin B, aflatoxin B content and the degree of medicinal mildew, but not directly proportional . 3.2 The experiment had projected a water a methanol-acetonitrile (63:26:11), acetonitrile and water (35:65), methanol water (9:1) mobile phase, such as testing, aflatoxin B, the separation are poor, by trial and error to determine the chromatographic conditions used in this experiment is the best, aflatoxin B and other components can get a better peak separation. 3.3 through extensive literature review found that aflatoxin B, the detection method more, but the application of high performance liquid chromatography with UV detector aflatoxin B, study less, and almost all of the high performance liquid chromatography are equipped with UV detector, so the medicines established in this study of aflatoxin B, Determination, accurate, reliable, easy to popularize. For aflatoxin other structures (B:, M, M, G, G to be further study. References: [1] Wu Kun and so on. Nutrition and Food Hygiene. Fifth Edition. People's Health Press,[link widoczny dla zalogowanych], 224. [2] Ye Xue beads. Detection of aflatoxin B analysis. Food and Fermentation Industries. 2003,29 (10) :90-92. [3] Chinese National Standards GB/T5009-2003. Food in the determination of aflatoxin B method. 101-107
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