GC测定二-(2,6-二氟苯甲酰异羟肟酸)二正丁基合锡中有机溶剂残留量

Determination of Residual Organic Solvents in Di--butyl-(2,6-difluorobenzohydroxamato) Tin(IV) by GC

关键词:  毛细管气相色谱法  二-(2,6-二氟苯甲酰异羟肟酸)二正丁基合锡  有机溶剂残留

Key words:  capillary gas chromatography  Di--butyl- (2,6-difluorobenzohydroxamato) Tin(IV)  residual organic solvents

摘要:

目的 建立原料药二-(2,6-二氟苯甲酰异羟肟酸)二正丁基合锡中的有机溶剂残留量的测定方法。方法 采用毛细管气相色谱法，FID检测器，DB-1毛细管柱，柱温50 ℃，进样口温度200 ℃，检测器温度220 ℃，流速为2.0 mL·min^-1，分流比为50∶1，以1,2-二氯乙烷为内标测定溶剂残留量。结果 甲醇、正己烷、甲苯在考察的浓度范围内线性关系良好，线性范围分别为9~375 μg·mL^-1(r=0.999 8)，0.87~36.25 μg·mL^-1(r=0.999 7)，2.67~111.25 μg·mL^-1(r=0.999 8)，平均回收率分别为99.1%(RSD=2.5%)、98.3%(RSD=2.7%)、99.7%(RSD=1.3%)。结论 本方法快速、简单、结果准确，可用于二-(2,6-二氟苯甲酰异羟肟酸)二正丁基合锡中的有机溶剂残留量的测定。

Abstract:

OBJECTIVE To develop a method for the determination of residual organic solvents in Di-n-butyl- (2,6-difluorobenzohydroxamato)Tin(IV). METHODS The capillary gas chromatography method was established with FID detector and DB-1 capillary column with 50 ℃. The temperature at the injector and the detector were 200 ℃ and 220 ℃, respectively. The carrier gas was nitrogen with a flow rate of 2.0 mL·min^-1. The split ratio was 50∶1. The 1,2-dichloroethane was used as the internal standard to determine the residual organic solvents. RESULTS Methanol, N-hexane and methylbenzene showed a linear range within 9-375 μg·mL^-1(r=0.999 8), 0.87-36.25 μg·mL^-1(r=0.999 7), 2.67-111.25 μg·mL^-1 (r=0.999 8), respectively. The average recoveries were 99.1%(RSD=2.5%), 98.3%(RSD=2.7%), 99.7%(RSD=1.3%), respectively. CONCLUSION The method was rapid, simple, accurate and suitable for the analysis of residual organic solvents in Di-n-butyl- (2,6-difluorobenzohydroxamato) Tin(IV).