提出采用近红外光谱技术(Near infrared spectra,NIR)快速测定抗癌药紫杉醇注射液中紫杉醇含量的方法,实现医院药房对注射液使用前的再测定。对24个月内生产的不同批次的紫杉醇注射液,通过透射方式测定其在12000～4000cm-1的近红外吸收光谱,采用偏最小二乘算法(Partial least-squares,PLS)建立了校正模型,通过不同光谱预处理、维数、波数范围进行组合筛选。当采用减去一条直线,维数为6,波数范围为9002.5～4597.7cm-1时能最有效地提取光谱中的有效信息校正集标准偏差(Standard error of the calibration sets,SEC)为0.035,预测集标准偏差(Standard error of the prediction sets,SEP)为0.059,预测集样品的百分偏差都在±2%以内。该方法快速简便,适合于医院药房常用重要药品的快速测定分析。
To develop a fast and sensitive liquid chromatography-mass spectrometry method for the determination of penehyclidine hydrochloride （PH） in beagle dog plasma. PH and diphenhydramine hydrochloride （internal standard, IS） were extracted with a solvent mixture of petroleum ether-ethyl ether （7：3）. Chromatographic separation was achieved on a reversed-phase Eclipse XDB-C18 column （4.6 mm × 150 mm, 5 um） using the eluent of methanol-water （5 mmol/L ammonium acetate） （90：10, v/v, pH 5.8） as mobile phase. The electrospray ionization source was set at the positive multiple reaction monitoring （MRM） mode. This method involved the use of the [M＋H]^＋ ions of PH and diphenhydramine hydrochloride at m/z 316.4- 128.2 and m/z 256.4-167.2. The calibration curve was linear in the range of 1-1000 ng/mL with a correlation coefficient of 0.9988. The lower limit of quantification was 0.05 ng/mL. The precision, accuracy and recovery of the method were acceptable. Following intravenous injection admires＇ tration at doses of 0.5, 1 and 5 mg/kg PH, the main pharmacokinetic parameters were as the followings, t1/2a 0.33 h, t1/2β 2.44 1% tmax 0.058 1% AUC and Cmax exhibited a linear increase along with the increase of dose. The two-compartment model fit the three dose groups. This method was sensitive, accurate and fast for the determination of concentration of PH in beagle dog plasma. It could be used in pharmacokinetic studies of PH.
