离子色谱法测定盐酸吉西他滨药品中的氟

Determination of total fluorine in gemcitabine hydrochloride by ion chromatography

分别用过硫酸钾湿消解法、过硫酸钾加压湿消解法、双氧水加压湿消解法、干灰化法对盐酸吉西他滨进行氧化处理,将有机氟转化为无机氟,用离子色谱法测定氟离子含量,间接测得盐酸吉西他滨中的总氟量。实验考量了过硫酸钾、氢氧化钠和双氧水的用量。在选择的样品预处理方法和色谱条件下,后3种方法转化率达到88.9%～98.6%,回收率为89.4%～105%,在此基础上,建立了盐酸吉西他滨药品中总氟的定量测定方法,F-含量在0.1～10 mg/L的浓度范围内呈线性,线性回归系数为0.9996,相对标准偏差为2.4%,检测限为0.01 mg/L。

Total fluorine in Gemcitabine hydrochloride was oxidized to fluoride ion by potassium persulfate-wet decomposition, potassium persulfate, pressurized wet decomposition, hydrogen peroxide, pressurized wet decomposition and dry cineration, Fluoride ion was determined by using ion chromatography for indirect measurement of total fluorine in Gemcitabine hydrochloride. The dosage of K2S2O8 , NaOH and H2O2 were discussed. The results showed conversion rate of that three methods reached 88.9% ~ 98.6% and the recoveries reached 89.4% -105% under the afore mentioned, Based on this, a method for the quantification of the F- concentration for indirect measurement of total fluorine in Gemcitabine hydrochloride was developed, When the concentration of fluoride ion was in the range from 0. 1 mg/L to 10 mg/L, the regression coefficient was 0. 9996. The relative standard deviation of fluoride ion is 2.4%, and the detection limit is 0. 01 mg/L.