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目的建立明胶空心胶囊中的铬的形态检测方法。方法以0.25 mmol/L乙二胺四乙酸二钠-2 mmol/L四丁基氢氧化铵-5%甲醇为流动相,经Agilent Eclipse XDB-C18(3.0 mm×150 mm,5μm)色谱柱分离,微波提取反相离子对色谱分离电感耦合等离子体质谱完成明胶空心胶囊中的Cr(Ⅲ)和Cr(Ⅵ)测定。结果水微波提取和分析过程中Cr(Ⅲ)和Cr(Ⅵ)不相互转化,三价铬由于没有形成络阴离子,不会形成色谱峰,此时只能测定Cr(Ⅵ),用乙二胺四乙酸二钠提取时,三价铬与之形成络阴离子,进而形成色谱峰,此时有部分六价铬转化为三价铬,根据峰面积计算出此时三价六价铬的含量总值,减去用水提取出的六价铬,即可得到三价铬真实含量。Cr(Ⅲ)、Cr(Ⅵ)检出限分别为0.6和0.51 mg/kg,线性范围:5~100μg/L。结论本方法能使用于明胶空心胶囊中铬形态的测定。
Objective To establish a method for the determination of chromium in gelatin hollow capsules. Methods 0.25 mmol / L disodium edetate-2 mmol / L tetrabutylammonium hydroxide-5% methanol was used as the mobile phase and separated by Agilent Eclipse XDB-C18 column (3.0 mm × 150 mm, 5 μm) Determination of Cr (Ⅲ) and Cr (Ⅵ) in Gelatin Hollow Capsules by Reversed-phase Ion-pair Chromatography with Inductively Coupled Plasma Mass Spectrometry. Results Cr (Ⅲ) and Cr (Ⅵ) did not transform into each other during microwave extraction and analysis. Chromium (Ⅵ) could not be formed due to the absence of complex anions and trivalent chromium. Tetraacetate disodium extraction, trivalent chromium with the formation of complex anions, and then the formation of chromatographic peaks, at this time some of the hexavalent chromium into trivalent chromium, calculated according to the peak area of trivalent hexavalent chromium total content , Minus the hexavalent chromium extracted with water, you can get the true content of trivalent chromium. The detection limits of Cr (Ⅲ) and Cr (Ⅵ) were 0.6 and 0.51 mg / kg, respectively. The linear range was 5-100 μg / L. Conclusion This method can be used to determine the chromium form in gelatin hollow capsules.