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目的建立液相色谱-质谱法测定保健食品中总铬、三价铬及六价铬含量的分析方法,并与原子吸收法的检测结果进行比较。方法利用液相色谱-质谱法测定提取和氧化反应前后样品溶液中六价铬,分别计算总铬、三价铬和六价铬的量。结果 8批样品(3批胶囊,5批片剂)测定六价铬和总铬含量分别为188.7~257.8mg/kg和189.1~257.4 mg/kg。该方法可以实现保健食品中总铬、三价铬和六价铬的测定,六价铬的方法检出限为0.03 mg/kg,RSD=3.72%(n=5),定量限为1.0 mg/kg,RSD=3.07%(n=5)。结论该方法简便易行,与原子吸收法测定总铬的结果一致,可用于保健食品中铬及其形态的测定。
OBJECTIVE To establish a method for the determination of total chromium, trivalent chromium and hexavalent chromium in health food by liquid chromatography-mass spectrometry and to compare with the results of atomic absorption spectrometry. Methods The contents of hexavalent chromium in the sample solution before and after the extraction and oxidation were determined by liquid chromatography-mass spectrometry. The contents of total chromium, trivalent chromium and hexavalent chromium were calculated respectively. Results The contents of hexavalent chromium and total chromium in 8 batches of samples (3 batches of capsules and 5 batches of tablets) were 188.7-257.8 mg / kg and 189.1-2557.4 mg / kg, respectively. The method can be used for the determination of total chromium, trivalent chromium and hexavalent chromium in health food. The detection limit of hexavalent chromium is 0.03 mg / kg, RSD = 3.72% (n = 5), the limit of quantification is 1.0 mg / kg, RSD = 3.07% (n = 5). Conclusion The method is simple and easy to use, consistent with the results of atomic absorption spectrometry for determination of total chromium. It can be used for the determination of chromium and its forms in health food.