气相色谱法同时测定拉西地平原料药中4种有机溶剂的残留量 点击下载
论文标题: 气相色谱法同时测定拉西地平原料药中4种有机溶剂的残留量
英文标题:
中文摘要: 目的: 建立同时测定拉西地平原料药中乙醇、二氯甲烷、异丙醇、乙酸乙酯4 种有机溶剂残留量的方法。方法:采用气相色谱法。色谱柱为DB-624毛细管柱,程序升温,检测器为氢火焰离子化检测器,检测器温度为250 ℃,载气为氮气,流速为2.0 mL/min,分流比为10 ∶ 1,进样量为1.0 μL。结果:乙醇、二氯甲烷、异丙醇、乙酸乙酯检测质量浓度线性范围分别为0.259 5~2.076 mg/mL(r=0.999 6)、0.055 3~0.316 mg/mL(r=0.999 2)、0.342 3~1.956 mg/mL(r=0.999 5)、0.370 6~2.118 mg/mL(r=0.999 4);定量限分别为2.96、2.24、4.4、4.44 μg/mL,检测限分别为0.887、0.672、1.3、1.32 μg/mL;精密度、稳定性、重复性试验的RSD<4.0%;加样回收率分别为 95.00%~101.17%(RSD=2.19%,n=9)、96.22%~104.53%(RSD=3.27%,n=9)、96.20%~104.90%(RSD=2.41%,n=9)、95.60%~104.48%(RSD=2.85%,n=9)。结论: 该方法简单、灵敏、可靠,适用于拉西地平原料药中4种有机溶剂残留量的同时测定。
英文摘要: OBJECTIVE: To establish a method for simultaneous determination of 4 residual organic solvents such as ethanol, dichloromethane, isopropanol and ethyl acetate in lacidipine raw material. METHODS: GC method was adopted. The determination was performed on DB-624 capillary column at the rate of 2.0 mL/min using nitrogen gas as carrier and FID as the detector by temperature programming. The temperature of detector was set at 250 ℃. Carries gas was nitrogen. The split ratio was 10 ∶ 1. The sample size was 10 μL. RESULTS: The linear ranges of ethanol, dichloromethane, isopropanol and ethyl acetate were 0.259 5-2.076 mg/mL (r=0.999 6), 0.055 3-0.316 mg/mL (r=0.999 2), 0.342 3-1.956 mg/mL (r=0.999 5), 0.370 6-2.118 mg/mL(r=0.999 4), respectively. The limits of quantification were 2.96, 2.24, 4.4, 4.44 μg/mL, and the detection limits were 0.887,0.672,1.3,1.32 μg/mL, respectively. RSDs of precision, stability and reproducibility tests were all lower than 4.0%. The recoveries were 95.00%-101.17%(RSD=2.19%,n=9), 96.22%-104.53%(RSD=3.27%,n=9), 96.20%-104.90%(RSD=2.41%,n=9), 95.60%-104.48%(RSD=2.85%,n=9). CONCLUSIONS: The method is simple, sensitive and reliable, and is suitable for simultaneous determination of 4 residual organic solvents in lacidipine raw material.
期刊: 2017年第28卷第30期
作者: 杜霞,王爱华,寻延滨
英文作者: DU Xia,WANG Aihua,XUN Yanbin
关键字: 拉西地平;气相色谱法;残留溶剂;乙醇;二氯甲烷;异丙醇;乙酸乙酯
KEYWORDS: Lacidipine; GC; Residual solvents; Ethanol; Dichloromethane; Isopropanol; Ethyl acetate
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