替代基质顶空气相色谱法测定健儿清解液中游离氢氰酸的含量

Quantitation of Free Hydrogen Cyanide in Jian’er Qingjie Mixture by Headspace Gas Chromatography Using a Surrogate Matrix Approach

关键词:  健儿清解液  顶空气相色谱  游离氢氰酸  替代基质

Key words:  Jian’er Qingjie mixture  headspace gas chromatography  free hydrogen cyanide  surrogate matrix

摘要:

目的 建立顶空进样气相色谱法测定健儿清解液中游离氢氰酸的含量。方法 采用Agilent PLOT-Q毛细管柱(30 m×0.32 mm，40 µm)，进样口温度200 ℃，分流比为5∶1，柱温箱程序升温，FID检测器温度为300 ℃；使用HPLC评估顶空加热过程中样品内氢氰酸前体化合物杏仁腈的稳定性，优化顶空平衡温度为50 ℃，平衡时间30 min；为降低基质效应的影响，以0.10 g·mL^-1的氯化钠溶液为替代基质，配制替代基质标准曲线。结果 氢氰酸在0.519~20.775 μg·mL^-1内与峰面积线性关系良好(r=1.000 0)；平均加样回收率为96.7%，RSD为2.6%(n=9)；替代基质标准曲线法与标准加入法的测定结果相对偏差<7%；5家企业生产的10批次样品中游离氢氰酸的含量为0.653~16.540 μg·mL^-1。结论 该方法简单、准确，可以用于健儿清解液的质量控制及安全性评价。

Abstract:

OBJECTIVE To establish a method for quantitation of free hydrogen cyanide in Jian’er Qingjie mixture by headspace gas chromatography.METHODS The assay was performed on an Agilent PLOT-Q capillary column(30 m×0.32 mm, 40 µm) combined with an oven temperature program. The GC injection port was maintained at 200 ℃ and the split ratio was 5∶1. The temperature for FID detector was set at 300 ℃. Samples were incubated at 50 ℃ for 30 min before headspace sampling and injection according to the stability evaluation of mandelonitrile which the unstable coexisting precursor of hydrogen cyanide by HPLC after incubation under different temperature conditions. The standard curves were prepared using 0.10 g·mL^-1 sodium chloride solution as surrogate matrix to overcome matrix effects. RESULTS The linear range of hydrogen cyanide was 0.519-20.775 µg·mL^-1(r=1.000 0). The average recovery was 96.7% with RSD of 2.6%(n=9). The relative deviation of the measurement results of the alternative matrix standard curve method and the standard addition method was <7%. The content range of free hydrogen cyanide in the 10 batches of Jian’er Qingjie mixture produced by 5 manufactures was 0.653-16.540 µg·mL^-1. CONCLUSION The established method is simple, accurate and reproducible. It can be useful for the quality control and safety evaluation of Jian’er Qingjie mixture.