摘要
目的:建立同时测定保泰松原料药中6种溶剂残留量的方法。方法:采用顶空气相色谱法。色谱柱为Agilent HP-5毛细管柱,程序升温,进样口温度为200℃,检测器为氢火焰离子化检测器,温度为250℃,载气为氮气(纯度:99.99%),载气流速为2.0 mL/min,分流比为5∶1,顶空平衡温度为60℃,顶空平衡时间为30 min,顶空进样量为1 mL。结果:甲醇、乙醇、异丙醇、二氯甲烷、乙酸乙酯和N,N-二甲基甲酰胺检测质量浓度线性范围分别为0.15~4.5μg/mL(r=0. 999 9)、0.25~7.5μg/m L(r=0. 999 7)、0.25~7.5μg/mL(r=0. 999 7)、0.03~0.9μg/m L(r=0. 999 3)、0.25~7.5μg/mL(r=0. 999 3)、0.044~1.32μg/mL(r=0. 999 3);检测限分别为0.05、0.08、0.08、0.01、0.08、0.015μg/mL,定量限分别为0.15、0.25、0.25、0.03、0.25、0.044μg/mL;精密度试验的RSD<2.0%,稳定性、重复性试验的RSD<3.0%;加样回收率分别为98.75%~100.12%(RSD=0.56%,n=9)、98.07%~101.20%(RSD=1.12%,n=9)、98.36%~100.80%(RSD=0.92%,n=9)、98.33%~101.67%(RSD=0.98%,n=9)、98.11%~100.40%(RSD=0.72%,n=9)、98.75%~101.05%(RSD=0.89%,n=9)。结论:该方法操作简便、准确,精密度、稳定性、重复性、耐用性好,可用于保泰松原料药中6种溶剂残留量的同时测定。
OBJECTIVE:To establish a method for simultaneous determination of residual solvents in phenylbutazone raw material. METHODS:Head-space GC was adopted. The determination was performed on Agilent HP-5 capillary column by temperature programming. The temperature of injector was 200 ℃,and detector was flame ionization detector with temperature of250 ℃;carrier gas was nitrogen(purity:99.99%)at the flow rate of 2.0 mL/min. The split ratio was 5 ∶1. Headspace equilibrium temperature was 60 ℃,and equilibration time was 30 min. The sample size was 1 mL. RESULTS:The linear range was 0.15-4.5μg/mL for methanol(r=0.999 9),0.25-7.5 μg/mL for ethanol(r=0.999 7),0.25-7.5 μg/mL for isopropyl alcohol(r=0.999 7),0.03-0.9 μ g/mL for dichloromethane(r=0.999 3),0.25-7.5 μ g/m L for ethyl acetate(r=0.999 3),0.044-1.32 μ g/m L for N,N-dimethyl formamide(r=0.999 3),respectively. The limits of detection were 0.05,0.08,0.08,0.01,0.08,0.015 μg/m L. The limits of quantitation were 0.15,0.25,0.25,0.03,0.25,0.044 μ g/mL. RSDs of precision test were lower than 2.0%. RSDs of stability and reproducibility tests were lower than 3.0%. The recoveries were 98.75%-100.12%(RSD=0.56%, n=9),98.07%-101.20%(RSD=1.12%,n=9),98.36%-100.80%(RSD=0.92%,n=9),98.33%-101.67%(RSD=0.98%,n=9),98.11%-100.40%(RSD=0.72%,n=9)and 98.75%-101.05%(RSD=0.89%,n=9). CONCLUSIONS:The method is simple,accurate,precise,stable,reproducible and durable,and can be used for simultaneous determination of 6 residual solvents in phenylbutazone raw material.
引文
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