Banerjee S, Chattopadhyay P, Ghosh A, Kaity S, Veer V
Division of Pharmaceutical Technology, Defence Research Laboratory, Tezpur, Assam, India.
Drug Res (Stuttg). 2013 Sep;63(9):450-6. doi: 10.1055/s-0033-1343471. Epub 2013 Apr 30.
In the present study, a simple, precise, specific, fast, accurate and reliable reverse phase high performance liquid chromatographic (RP-HPLC) method has been developed and validated for the simultaneous determination and quantification of eserine and pralidoxime chloride in drugs-in-adhesive matrix type transdermal patches.
The chromatographic separation was achieved by C18 column, using a mobile phase consisting of acetonitrile: 10 mM potassium dihydrogen phosphate, 10 mM heptane-1-sulfonic acid sodium salt monohydrate in water (30:70, v/v) adjusted at pH 3.0 with ortho-phosphoric acid. Flow rate was 1.0 mL/min and UV detection at 238 nm. The method was validated according to the International Conference on Harmonization (ICH) guidelines.
The calibration curves were linear over the different concentration ranges of 0.5-10 μg/ml for eserine and 5-25 μg/mL for 2PAM. Relative standard deviation for precision was less than 2.0%. Limit of detection values of eserine and 2-PAM were 0.018 µg/mL and 0.008 µg/mL, respectively. The limit of quantification of eserine and 2-PAM were 0.055 µg/mL and 0.026 µg/mL, respectively.
The developed method was applied for the routine analysis of these 2 drugs in drugs-in-adhesive matrix type transdermal patches in order to evaluate the drug content of different formulations. It could be also used with reliability for the determination of the drug in other pharmaceutical dosage forms.
在本研究中，已开发并验证了一种简单、精确、特异、快速、准确且可靠的反相高效液相色谱（RP-HPLC）方法，用于同时测定和定量分析药物贴剂基质型透皮贴剂中的毒扁豆碱和氯解磷定。
采用C18柱进行色谱分离，流动相由乙腈：10 mM磷酸二氢钾、10 mM一水合庚烷-1-磺酸钠盐的水溶液（30:70，v/v）组成，用正磷酸调节pH值至3.0。流速为1.0 mL/min，在238 nm处进行紫外检测。该方法根据国际协调会议（ICH）指南进行了验证。
毒扁豆碱在0.5-10 μg/ml的不同浓度范围内校准曲线呈线性，氯解磷定在5-25 μg/mL范围内校准曲线呈线性。精密度的相对标准偏差小于2.0%。毒扁豆碱和氯解磷定的检测限分别为0.018 µg/mL和0.008 µg/mL。毒扁豆碱和氯解磷定的定量限分别为0.055 µg/mL和0.026 µg/mL。
所开发的方法用于药物贴剂基质型透皮贴剂中这两种药物的常规分析，以评估不同制剂的药物含量。它也可可靠地用于其他药物剂型中药物的测定。
