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目的建立注射用替曲朵辛盐酸利多卡因的含量及有关物质检测方法。方法采用高效液相色谱法,替曲朵辛的检测条件为:ZORBAX SB-C8柱(4.6mm×250mm,5μm),流动相为辛烷磺酸钠的磷酸盐缓冲液,流速0.3mL·min~(-1),激发波长365nm,发射波长510nm,柱后衍生剂为4mol·L~(-1)氢氧化钠溶液,衍生剂流速0.3mL·min~(-1),柱后衍生温度110℃,进样量50μL;盐酸利多卡因的检测条件为:TECHMaTe C18-STⅢ柱(4.6mm×250mm,5μm),流动相为磷酸盐缓冲液-乙腈(50∶50),流速1mL·min~(-1),柱温30℃,紫外检测波长254nm,进样量5μL。结果替曲朵辛和盐酸利多卡因的线性范围分别为0.102 4~10.24μg·mL~(-1)和0.501 0~15.032 4 mg·mL~(-1);平均回收率分别为100.48%和99.78%,RSD分别为1.13%和0.65%(n=9);检测限分别为0.41ng·mL~(-1)和10.3μg·mL~(-1),定量限分别为0.81ng·mL~(-1)和28.5μg·mL~(-1)。结论本方法可用于测定该制剂中替曲朵辛和盐酸利多卡因的含量及有关物质。
Objective To establish a method for the determination of lidotoxin hydrochloride lidocaine for injection and its related substances. Methods The HPLC conditions were as follows: ZORBAX SB-C8 column (4.6mm × 250mm, 5μm), the mobile phase was sodium octane sulfonate phosphate buffer, the flow rate was 0.3mL · min ~ (-1), the excitation wavelength was 365 nm, the emission wavelength was 510 nm, the column derivatization reagent was 4mol·L -1 sodium hydroxide solution, the flow rate of derivatizing agent was 0.3mL · min -1, the column derivatization temperature was 110 ℃, and the injection volume was 50μL. The detection conditions of lidocaine hydrochloride were: TECHMaTe C18-STⅢ column (4.6mm × 250mm, 5μm), the mobile phase consisted of phosphate buffer-acetonitrile (-1), column temperature 30 ℃, UV detection wavelength 254nm, injection volume 5μL. Results The linear ranges of tebutroxine and lidocaine hydrochloride were 0.102 4 ~ 10.24 μg · mL -1 and 0.501 0 ~ 15.032 4 mg · mL -1, respectively. The average recoveries were 100.48% and The detection limits were 0.41 ng · mL -1 and 10.3 μg · mL -1, respectively, and the limit of quantification were 0.81 ng · mL -1 and 99.78%, respectively, with RSDs of 1.13% and 0.65% (n = 9) (-1) and 28.5μg · mL -1. Conclusion This method can be used to determine the content of tegundotine hydrochloride and lidocaine hydrochloride in the preparation and related substances.