亲水作用色谱-质谱法检测牛磺酸颗粒中的牛磺酸  

Determination of taurine in taurine granules by HILIC-MS

作　　者：潘军 王颖臻 

机构地区：[1]滨州市食品药品检验检测中心,滨州256602

出　　处：《药物分析杂志》2016年第11期1999-2003,共5页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立牛磺酸颗粒中牛磺酸的含量测定方法。方法:采用亲水作用色谱-质谱法,以HYPERSIL APS-2(氨丙基)为色谱柱固定相,以0.1%甲酸水溶液为流动相A,乙腈为流动相B,进行梯度洗脱(0~10 min,90%B→80%B;10~15 min,90%B),流速为0.4 mL·min^(-1),柱温箱温度35.0℃,进样量1.0μL,单次运行时间为15 min;用ESI离子源,以m/z=+126.0选择离子监测模式进行质谱定量。结果:本分析条件下,牛磺酸颗粒中的牛磺酸可以实现较好的分离,且具有较高的分子离子丰度,牛磺酸质量浓度与峰面积在测定范围内线性关系良好(r=0.999 6);准确度良好,平均加样回收率在97.7%~100.7%之间,测定3批牛磺酸颗粒中含牛磺酸的量分别为标示量的100.6%、100.2%、100.7%。结论:经方法学验证,该方法可应用于牛磺酸颗粒中牛磺酸的含量测定。Objective： To establish a method for the determination of taurine content in taurine granules. Methods： The taurine was separated on an HYPERSIL APS-2 （ aminopropyl ） column by hydrophilic interaction chromatography （ HILIC ） combined with tandem-mass spectrometry. The mobile phase consisted of 0. 1% formic acid in water（ A ） and acetonitrile （ B ） in gradient elution mode （ 0-10 min, 90%B → 80%B; 10-15 min, 90%B ） at a flow rate of 0.4 mL. mm-1 . The column temperature was 35.0 ℃, the injected sample volume was 1.0 μ L, and the single run time was 15.0 min. ESI source was employed, and m/z=＋126.0 was picked in selective ionization monitoring （ SIM ） mode of mass spectrometry. Results： In the above mentioned analysis condition, the tanrine in taurine granules achieved a good separation and exhibited a higher abundance of molecular ion. The calibrated concentration curves of taurine were linear with the concentration range of determination （ r=0. 999 6 ）. The accuracy was good with average recoveries between 97. 7%-100. 7%. Compared with the labeled amount, the taurine contents of three batches of samples are 100.6%, 100.2%, and 100.7%, respectively. Conclusion： The established method is proved by methodology validation that it can be applied to the taurine determination in taurine granules.

关 键 词：牛磺酸 β-氨基乙磺酸 游雕氨基酸 牛磺酸颗粒 含量测定 离子监测模式 亲水作用色谱-质谱 

分 类 号：R917[医药卫生—药物分析学]