顶空气相色谱法检测原料药氯沙坦钾中的残留溶剂

Determination of Residual Solvents in Losartan Potassium by Head Space Gas Chromatography

关键词:  气相色谱法  顶空  原料药  氯沙坦钾  残留溶剂

Key words:  gas chromatography  head space  active pharmaceutical ingredients  losartan potassium  residual solvents

摘要:

目的 建立顶空气相色谱法测定氯沙坦钾原料药有机残留溶剂的方法。方法 选用Agilent 7890气相色谱仪，配备7697顶空进样器，DB-624毛细管色谱柱作为分析柱，FID检测器，外标法测定；并对分析方法建立进行研究。结果 甲醇、异丙醇、乙酸乙酯、环己烷、甲苯分别在0.122~90.2，0.28~151.3，0.03~61.4，0.22~76.4，0.035~26.8 μg·mL^-1线性关系良好（r>0.999）；各组分检测限分别为0.037，0.090，0.009，0.070，0.012 μg·mL^-1；各组分平均回收率为90.0%~110.0%。结论 该方法简单、可靠、准确，可用于原料药氯沙坦钾有机残留溶剂的测定。

Abstract:

OBJECTIVE To establish a head space gas chromatography method for determination of residual solvents in active pharmaceutical ingredients of losartan potassium.METHODS Agilent 7890 gas chromatography with 7697 head space sampling and FID detector was selected.And DB-624 capillary column was used as analytical column.External standard method was used to determine the content.The analytical method was also explored.RESULTS A good linear correlation of methanol,isopropanol,ethyl acetate,cyclohexane and toluene were showed at the range of 0.122-90.2,0.28-151.3,0.03-61.4,0.22-76.4 and 0.035-26.8 μg·mL^-1 with r>0.999,respectively.Detection limit of each components was 0.037,0.090,0.009,0.070,0.012 μg·mL^-1,respectively;Recovery range was 90.0%-110.0%.CONCLUSION The method is simple,reliable and accurate,can be used for determination of preservatives and sweeteners in oral liquid preparation.