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二维超高效液相色谱-飞行时间质谱联用技术鉴定氯化琥珀胆碱原料药中的杂质
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| 篇名： | 二维超高效液相色谱-飞行时间质谱联用技术鉴定氯化琥珀胆碱原料药中的杂质 |
| TITLE： | |
| 摘要： | 目的：建立鉴定氯化琥珀胆碱原料药中杂质的方法。方法：采用二维超高效液相色谱-飞行时间质谱联用技术。一维色谱柱为Hypersil GOLD C18，以缓冲液（含22 mmol/L戊烷磺酸钠+50 mmol/L氯化钠+5 mmol/L硫酸）为流动相A，以乙腈为流动相B，流动相A、B的体积比为95 ∶ 5，柱温为40 ℃，流速为1.0 mL/min，检测波长为214 nm；二维色谱柱为ACQUITY UPLC BEH C18，以0.1％氨水为流动相A，以乙腈为流动相B，采用梯度洗脱，柱温为30 ℃，流速为0.4 mL/min；离子化模式为ESI+，毛细管电压为2.5 kV，离子源温度为120 ℃，雾化气温度为450 ℃，雾化气流速为900 L/h，采集模式为MSE。结果：通过一维液相色谱在氯化琥珀胆碱原料药中检出琥珀酸、琥珀酰氯（工艺中间体）及吡啶（试剂）等杂质；另有4个比较明显的未知杂质，分别命名为杂质1、杂质2、杂质3、杂质4，其中尤以杂质2的表观含量最高。通过二维液相色谱质谱联用法推断杂质2为脱氢琥珀酰单胆碱，杂质4为氯化琥珀酰单胆碱，杂质1、杂质3在质谱中均未被检测到信号。结论：本研究建立了鉴定氯化琥珀胆碱原料药中杂质的方法，其研究结果可用于评价氯化琥珀胆碱原料药的质量。 |
| ABSTRACT： | OBJECTIVE： To establish the method for the identification of impurities in succinylcholine chloride raw material. METHODS： Two-dimensional UPLC-QTOF-MS was adopted. One dimension chromatographic condition was Hypersil GOLD C18 column using buffer solution （22 mmol/L sodium pentanesulfonate+50 mmol/L sodium chloride+5 mmol/L sulphuric acid） as mobile phase A and acetonitrile as mobile phase B， volume ratio of mobile phase A to mobile phase B 95 ∶ 5， column temperature of 40 ℃， flow rate of 1.0 mL/min， detection wavelength of 214 nm. Two-dimension chromatographic condition was ACQUITY UPLC BEH C18 column using 0.1％ ammonia as mobile phase A and acetonitrile as mobile phase B （gradient elution） with column temperature of 30 ℃ at flow rate of 0.4 mL/min. Ionization mode was ESI+ with capillary voltage of 2.5 kV， source temperature of 120 ℃， temperature of atomizing gas at 450 ℃， flow rate of atomizing gas at 900 L/h， acquisition mode of MSE. RESULTS： The succinic acid， succinyl chloride （intermediate）， pyridine （reagent） and other impurities were detected in succinylcholine chloride by one dimensional method of HPLC. Other 4 obvious unknown impurities were named impurity 1， impurity 2， impurity 3 and impurity 4， among which the apparent content of impurity 2 was the highest. Two-dimensional method of HPLC-QTOF-MS deduced that the impurity 2 was dehydrogenate succinylcholine chloride and impurity 4 was succinylcholine chloride. The impurity 1 and impurity 3 were not detected in mass spectrum. CONCLUSIONS： Establish method for the identification of impurity in succinylcholine chloride raw material， and the results of research are used for the evaluation of the quality of the succinylcholine chloride raw material. |
| 期刊： | 2018年第29卷第7期 |
| 作者： | 陈红，杨梅，张姮婕，袁铭，廉向金 |
| AUTHORS： | CHEN Hong，YANG Mei，ZHANG Hengjie，YUAN Ming，LIAN Xiangjin |
| 关键字： | 氯化琥珀胆碱；原料药；杂质；二维超高效液相色谱-飞行时间质谱联用技术 |
| KEYWORDS： | Succinylcholine chloride； Raw material； Impurity； Two-dimensional UPLC-QTOF-MS |
| 阅读数： | 320 次 |
| 本月下载数： | 15 次 |
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