Piekarski Mikołaj, Jelin'ska Anna, Szymczak Kamil
Pharmaceutical Chemistry, Karol Marcinkowski University of Medical Sciences, Poznań, Poland ; Inhospital pharmacy, Heliodor Swięcicki Clinical Hospital of PUMS, Poznań, Poland.
Eur J Hosp Pharm. 2012 Oct;19(5):447-451. doi: 10.1136/ejhpharm-2012-000088.
The use of a combination of different drugs in postoperative analgesia extends the time of analgesia, makes it more efficient and allows the use of lower drug doses, which leads to less risk of side effects and drug dependence. The aim of this study was to develop and validate an HPLC method to determine the stability of fentanyl citrate and bupivacaine hydrochloride mixtures in standard infusion solutions of 0.9% sodium chloride and 5% glucose.
AFTER OPTIMISATION, THE HPLC METHOD PARAMETERS WERE AS FOLLOWS: LiChrospher 100 CN, 250×4 mm (10 µm) column; mobile phase: mixture of acetonitrile and phosphate buffer at pH 2.8 (3:7, V/V) with addition of 0.08 g/l potassium chloride; flow rate: 1.5 ml/min; column temperature: 30°C; spectrophotometric detection at 210 nm. Development of the method involved checking the impact of acetonitrile and KCl concentrations in the mobile phase and choosing the internal standard. Method validation included determining the specificity of the method, its accuracy, linearity, precision, repeatability, limits of detection and quantification.
The retention times of bupivacaine hydrochloride, fentanyl citrate and procaine hydrochloride, used as an internal standard, were approximately 10 min, 15 min and 5 min, respectively. Method validation confirmed its selectivity, accuracy and precision. The average values of the variation and accuracy coefficients were 0.70% and 99.02% for bupivacaine hydrochloride, and 1.76% and 104.53% for fentanyl citrate. The intermediate precision values were 1.25% for bupivacaine hydrochloride and 1.52% for fentanyl citrate.
在术后镇痛中联合使用不同药物可延长镇痛时间，提高镇痛效果，并允许使用更低的药物剂量，从而降低副作用和药物依赖性风险。本研究的目的是开发并验证一种高效液相色谱（HPLC）方法，以测定枸橼酸芬太尼和盐酸布比卡因混合物在0.9%氯化钠和5%葡萄糖标准输注溶液中的稳定性。
优化后的HPLC方法参数如下：LiChrospher 100 CN，250×4 mm（10 µm）色谱柱；流动相：乙腈和pH 2.8的磷酸盐缓冲液（3:7，V/V）的混合物，并添加0.08 g/l氯化钾；流速：1.5 ml/min；柱温：30°C；在210 nm处进行分光光度检测。该方法的开发包括检查流动相中乙腈和氯化钾浓度的影响以及选择内标。方法验证包括确定方法的特异性、准确性、线性、精密度、重复性、检测限和定量限。
用作内标的盐酸布比卡因、枸橼酸芬太尼和盐酸普鲁卡因的保留时间分别约为10分钟、15分钟和5分钟。方法验证证实了其选择性、准确性和精密度。盐酸布比卡因的变异系数和准确性系数平均值分别为0.70%和99.02%，枸橼酸芬太尼的分别为1.76%和104.53%。盐酸布比卡因的中间精密度值为1.25%，枸橼酸芬太尼的为1.52%。
