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目的建立破壁灵芝孢子粉保健品中铅的湿法消解-石墨炉原子吸收测定方法,为保健食品质量控制提供检测依据。方法样品经硝酸-过氧化氢消化体系与硝酸-高氯酸消化体系消解,优化原子吸收分光光度仪的原子化和灰化升温程序,比较1%磷酸二氢铵和1%磷酸二氢铵-0.06%硝酸镁基体改进剂,将最佳的基体改进剂加入到样品消化液中,调整石墨炉原子吸收分光光度仪测定的最好状态后测定。结果测定浓度在0.0μg/L~50.0μg/L,方法的线性关系良好,相关系数r=0.999 5,检出限为0.14μg/L,相对标准偏差为4.6%~6.5%,样品的加标回收率为98%~110%。结论该方法具有操作简单、快速简便、灵敏度和准确度高的优点,具有较高的实用性,为有效控制破壁灵芝孢子粉保健品中铅提供了依据,便于推广应用。
Objective To establish a method for the determination of lead in wet health products of broken ganoderma lucidum spores by graphite furnace atomic absorption spectrometry and provide the basis for the quality control of health food. Methods The samples were digested by nitric acid - hydrogen peroxide digestion system and nitric acid - perchloric acid digestion system to optimize the atomization and ashing procedures of atomic absorption spectrophotometer. The comparison of 1% ammonium dihydrogen phosphate and 1% ammonium dihydrogen phosphate - 0.06% magnesium nitrate matrix modifier, the best matrix modifier was added to the sample digestion solution, adjusted by graphite furnace atomic absorption spectrophotometer to determine the best state after the determination. The linearity of the method was good with the concentration ranged from 0.0μg / L to 50.0μg / L. The correlation coefficient was 0.999 5, the detection limit was 0.14μg / L with the relative standard deviation of 4.6% -6.5%. The spiked samples The recovery rate is 98% ~ 110%. Conclusion The method has the advantages of simple operation, fast and easy, high sensitivity and accuracy, high practicability, and provides a basis for the effective control of lead in the broken health ganoderma lucidum spores and is convenient for popularization and application.