| 陈永强,洪碧红,易瑞灶.HPLC法测定注射用替曲朵辛盐酸利多卡因的含量及有关物质△[J].中国海洋药物,2016,35(3):67-75. |
| HPLC法测定注射用替曲朵辛盐酸利多卡因的含量及有关物质△ |
| HPLC determination contents and related substances in the tetrodotoxin lidocaine hydrochloride for injection |
| 投稿时间：2015-09-22 修订日期：2015-10-30 |
| DOI： |
| 中文关键词: 替曲朵辛 盐酸利多卡因 含量 有关物质 高效液相色谱法 |
| English Keywords:Tetrodotoxin Lidocaine hydrochloride Content Related substances |
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| 中文摘要: |
| 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（4.6 mm×250 mm，5 μm），流动相为辛烷磺酸钠的磷酸盐缓冲液，流速0.3 mLmin-1，激发波长365 nm，发射波长510 nm，柱后衍生剂为4 molL-1氢氧化钠溶液，衍生剂流速0.3 mLmin-1，柱后衍生温度110℃，进样量50 μL；盐酸利多卡因的检测条件为：TECHMaTe C18-STII柱（4.6 mm×250 mm，5 μm），流动相为磷酸盐缓冲液-乙腈（50:50），流速1 mLmin-1，柱温30℃，紫外检测波长254 nm，进样量5 μL。结果 替曲朵辛和盐酸利多卡因的线性范围分别为0.1024～10.24 μgmL-1和0.5010～15.0324 mgmL-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0.41 ngmL-1和10.3 μgmL-1，定量限分别为0.81 ngmL-1和28.5 μgmL-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。 |
| English Summary: |
| Objective: To establish an HPLC method for determining the contents and related substances of tetrodotoxin and lidocaine hydrochloride in the tetrodotoxin lidocaine hydrochloride for injection. Methods: The analysis of tetrodotoxin was performed on a ZORBAX SB-C8 column (4.6 mm×250 mm，5 μm) , using a mobile phase of phosphate buffer solution of octane sulfonate at the flow rate of 0.3 mLmin-1. The excitation wavelength and emission wavelength were set at 356 nm and 510 nm , respectively. The post column derivative reagent was 4 molL-1 NaOH at the flow rate of 0.3 mLmin-1，the post column derivatization temperature was maintained at 110℃ and injection volumn was 50 μL. The analysis of lidocaine hydrochloride was performed on a TECHMaTe C18-STII column (4.6 mm×250 mm，5 μm) , using a mobile phase of phosphate buffer-acetonitrile (50:50) at the flow rate of 1.0 mLmin-1. The column temperature was maintained at 30℃. The detection wavelength was set at 254 nm and injection volumn was 5 μL. Results: The linear ranges of tetrodotoxin and lidocaine hydrochloride were 0.1024-10.24 μgmL-1 and 0.5010-15.0324 mgmL-1 , respectively. The average recoveries of tetrodotoxin and lidocaine hydrochloride were 100.48% and 99.78%, respectively. The RSDs of this method were all less than 2% (n=9). The limit of detection of tetrodotoxin and lidocaine hydrochloride were 0.41 ngmL-1 and 10.3 μgmL-1, respectively. And the limit of quantitation of tetrodotoxin and lidocaine hydrochloride were 0.81 ngmL-1 and 28.5 μgmL-1, respectively.
Conclusion：The method is applicable for the contents and related substances control of tetrodotoxin lidocaine hydrochloride for injection.
Key words: Tetrodotoxin ；Lidocaine hydrochloride ；Content ；Related substances ； |
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