| 引用本文: | 邵天舒,郭雷,周长明.邻苯二甲醛柱前衍生化-HPLC测定复方氨基酸注射液中蛋氨酸亚砜的含量[J].中国现代应用药学,2018,35(4):497-500. |
| SHAO Tianshu,GUO Lei,ZHOU Changming.Determination of Methionine Sulfoxide in Compound Amino Acid Injection by HPLC with OPA Pre-column Derivatization[J].Chin J Mod Appl Pharm(中国现代应用药学),2018,35(4):497-500. |
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| 摘要: |
| 目的 建立测定复方氨基酸注射液中蛋氨酸亚砜含量的方法。方法 采用邻苯二甲醛（O-phthaladehyde，OPA）柱前衍生HPLC。色谱柱为Agilent ZORBAX Eclipse AAA C18柱（150 mm×4.6 mm，5µm），检测波长为338 nm，流动相A为0.04 mol·L-1磷酸二氢钠溶液（调节pH至7.8），流动相B为乙腈-甲醇-水（45：45：10），梯度洗脱，流速为2.0 ml·min-1，柱温为40℃，供试品溶液与OPA衍生剂及硼酸盐缓冲液按设定程序自动混匀后进样。结果 蛋氨酸亚砜的质量浓度线性范围为0.000 5~0.050 0 mg·mL-1（R=0.999 9）；定量限为0.250 5 μg·mL-1，检测限为0.083 5 μg·mL-1；精密度、稳定性、重复性试验的RSD<3.0%；平均回收率为99.1%（RSD=1.33%，n=9）。结论 该方法操作简便，可用于复方氨基酸注射液中蛋氨酸亚砜的含量测定。 |
| 关键词: 邻苯二甲醛 柱前衍生 高效液相色谱 复方氨基酸注射液 蛋氨酸亚砜 |
| DOI：10.13748/j.cnki.issn1007-7693.2018.04.009 |
| 分类号:R917.101 |
| 基金项目: |
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| Determination of Methionine Sulfoxide in Compound Amino Acid Injection by HPLC with OPA Pre-column Derivatization |
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SHAO Tianshu1,2, GUO Lei1,2, ZHOU Changming1,2
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1.Beijing Institute of Drug Control, Beijing 102206, China;2.Beijing Key Laboratory of Analysis and Biological Evaluation of Chinese Medicine, Beijing 102206, China
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| Abstract: |
| OBJECTIVE To establish a method for the content determination of methionine sulfoxide in Compound Amino Acid injection. METHODS O-phthaladehyde(OPA) pre-column derivatization HPLC was performed on the column of Agilent ZORBAX Eclipse AAA C18(150 mm×4.6 mm, 5 µm) with mobile phase A 0.04 mol·L-1 sodium dihydrogen phosphate solution (adjust pH to 7.8), mobile phase B acetonitrile-methanol-water (45:45:10)(gradient elution) at the flow rate of 2.0 ml·min-1, the detection wavelength was 338 nm and the column temperature was 40℃. The sample solution was automatic mixed with OPA agent and borate buffer according to set procedure. RESULTS The linear range of methionine sulfoxide was 0.000 5-0.050 0 mg·mL-1(R=0.999 9). The limit of quantitation was 0.250 5 μg·mL-1, and the limit of detection was 0.083 5 μg·mL-1. RSDs of precision, stability and repetitive test were all <3.0%. The average recovery was 99.1%(RSD=1.33%, n=9). CONCLUSION The method is simple, rapid and suitable for the content determination of methionine sulfoxide in Compound Amino Acid injection. |
| Key words: O-phthaladehyde(OPA) pre-column derivatization HPLC Compound Amino Acid injection methionine sulfoxide |
