目的:建立羟丙基二淀粉磷酸酯(HPDSP)中基因杂质氯丙醇检测方法。方法:使用气相色谱-质谱联用仪(GC-MS),采用Agilent VF-WAX毛细管色谱柱,柱温为程序升温(起始温度为80 ℃,保持8 min,再以35 ℃·min-1的速率升至220 ℃,保持5 min),流速2 mL·min-1,进样口温度200 ℃,不分流进样,进样量1 μL。检测器为电子轰击源(EI)质谱检测器,离子源温度为230 ℃,检测模式为选择性离子监测(SIM),1-氯-2-丙醇定性离子的m/z为45、43、79、81,定量离子的m/z为79,2-氯-1-丙醇定性离子的m/z为58、62、63、64、65,定量离子的m/z为62。结果:1-氯-2-丙醇质量浓度在20.04~1 002 ng·mL-1范围内线性关系良好(r=0.999 8,n=7);回收率为93.7%~117.1%;9批样品检测出氯丙醇含量范围为0.000 006%~0.000 08%。结论:该方法的检测灵敏度高,精密度好,准确度高,线性关系良好,可用于HPDSP中基因杂质氯丙醇的测定。
Objective: To establish a method for the detection of genetic impurity chloropropanol in hydroxypropyl distarch phosphate (HPDSP). Methods: The method was performed with Agilent VF-WAX capillary column and temperature programmed by GC-MS. The initial temperature was 80 ℃ for 8 min, then increased to 220 ℃ at the rate of 35 ℃·min-1 and maintained for 5 min with the flow rate of 2 mL·min-1. The temperature of inlet was 200 ℃, and the injection volume was 1 μL without split. The detector was electron impact (EI) with selected ion monitoring (SIM) mode and ion source temperature at 230 ℃. The m/z of qualitative ions of 1-chloro-2-propanol were 45, 43, 79, 81, and the m/z of quantitative ion was 79. The m/z of qualitative ions of 2-chloro-1- propanol were m/z 58, 62, 63, 64, 65, and m/z of the quantitative ion was 62. Results: Good linear was achieved in the range of 20.04 ng·mL-1 to 1 002 ng·mL-1 (r=0.999 8,n=7) and the recovery rate ranged from 93.7% to 117.1% for 1-chloro-2-propanol. The contents of chloropropanol in 9 batches were within the range of 0.000 006%-0.000 08%. Conclusion: The method shows the advantages of high sensitivity, good accuracy, linearity and can be used for the detection of genetic impurities in HPDSP.
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