气相色谱法同时测定尼尔雌醇原料药中7种有机溶剂的残留量

Simultaneous Determination of Seven Residual Solvents in Nilethylenol Raw Material by GC

目的:建立同时测定尼尔雌醇原料药中甲醇、乙醇、乙腈、异丙醇、甲苯、四氢呋喃和乙酸乙酯残留量的方法。方法:采用气相色谱法。色谱柱为DB-WAX毛细管柱,检测器为氢火焰离子化检测器,分流比为5∶1,载气为氮气(纯度:99.999%),流速为1.0 mL/min,进样量为1μL,直接进样,固定相为键合交联聚乙二醇,升温程序为初始温度40℃,保持5 min,以10℃/min速率升温至90℃,再以5℃/min速率升温至200℃,进样口温度为220℃,检测器温度为230℃。结果:甲醇、乙醇、乙腈、异丙醇、甲苯、四氢呋喃和乙酸乙酯的检测质量浓度线性范围分别为0.24～12.00μg/mL(r=0.999 7)、0.40～20.00μg/mL(r=0.999 5)、0.033～1.64μg/mL(r=0.999 8)、0.40～20.00μg/mL(r=0.999 5)、0.071～3.56μg/mL(r=0.999 6)、0.058～2.88μg/mL(r=0.999 8)、0.40～20.00μg/mL(r=0.999 7);定量限分别为0.24、0.40、0.033、0.40、0.071、0.058、0.40μg/mL,检测限分别为0.08、0.10、0.01、0.13、0.02、0.02、0.13μg/mL;精密度、稳定性、重复性试验的RSD均小于2%;加样回收率分别为98.17%～100.48%(RSD=0.92%,n=9)、97.77%～101.30%(RSD=1.32%,n=9)、97.56%～100.85%(RSD=1.20%,n=9)、98.64%～100.92%(RSD=0.87%,n=9)、98.54%～100.62%(RSD=0.76%,n=9)、98.26%～100.00%(RSD=0.74%,n=9)、98.30%～100.59%(RSD=0.76%,n=9)。结论:该方法灵敏度较高、准确度较好,可用于同时测定尼尔雌醇原料药中甲醇、乙醇、乙腈、异丙烷、甲苯、四氢呋喃和乙酸乙酯的残留量。

OBJECTIVE:To establish a method for simultaneous determination of residual methanol,ethanol,acetonitrile,isopropanol,methylbenzene,tetrahydrofuran and ethyl acetate in Nilethylenol raw material.METHODS:GC was performed.The determination was performed on DB-WAX capillary column.The detector was hydrogen flame ionization detector with split ratio of 5∶1.The carrier gas was nitrogen(purity:99.999% )at the flow rate of 1.0 mL/min.The sample size was 1μL,directly sampling with bonded crosslinked polyethylene glycol as stationary phase.The initial temperature was 40℃and was maintained for 5 min,increased to 90℃at 10℃/min,and then increased to 200℃at 5℃/min.The temperature of injector was 220℃,and detector temperature was 230℃.RESULTS:The linear range was 0.24-12.00μg/mL for methanol(r=0.999 7),0.40-20.00μg/mL for ethanol(r=0.999 5),0.033-1.64μg/mL for acetonitrile(r=0.999 8),0.40-20.00μg/mL for isopropanol(r=0.999 5),0.071-3.56μg/mL for methylbenzene(r=0.999 6),0.058-2.88μg/mL for tetrahydrofuran(r=0.999 8),0.40-20.00μg/mL for ethyl acetate(r=0.999 7),respectively.The limits of quantitation were 0.24,0.40,0.033,0.40,0.071,0.058,0.40μg/mL,respectively.The limits of detection were 0.08,0.10,0.01,0.13,0.02,0.02,0.13μg/mL,respectively.RSDs of precision,stability and reproducibility tests were all lower than 2% .The recoveries were 98.17% -100.48% (RSD=0.92% ,n=9),97.77% -101.30% (RSD=1.32% ,n=9),97.56% -100.85% (RSD=1.20% ,n=9),98.64% -100.92% (RSD=0.87% ,n=9),98.54% -100.62% (RSD=0.76% ,n=9),98.26% -100.00% (RSD=0.74% ,n=9),98.30% -100.59% (RSD=0.76% ,n=9),respectively.CONCLUSIONS:The method has high sensitivity and good accuracy,and can be used for the simultaneous determination of residual methanol,ethanol,acetonitrile,isopropane,methylbenzene,tetrahydrofuran and ethyl acetate in Nilethylenol raw material.