Yan Rui, Qu Longmei, Luo Nan, Liu Yang, Liu Yu, Li Li, Chen Lijiang
College of Pharmacy, Liaoning University, Shenyang 110036, China.
Yichang Humanwell Pharmaceutical Co., Ltd., Yichang 443005, China.
Int J Anal Chem. 2014;2014:841084. doi: 10.1155/2014/841084. Epub 2014 Dec 4.
Lactose is a widely used pharmaceutical excipient, sometimes irreplaceable. Traces of residual proteins left during production of lactose are potential allergen to body. The present paper describes a sensitive and specific LC-MS method for the determination of α-lactalbumin (α-La) in lactose samples. Chromatographic separation was performed on an Acquity UPLC BEH300 C18 column (2.1 × 150 mm, 1.7 μm) with an isocratic mobile phase consisting of water containing 0.1% TFA and acetonitrile containing 0.1% TFA (80 : 20, v/v). Mass spectrometric detection was achieved by a triple-quadrupole mass spectrometer equipped with an ESI interface operating in positive ionization mode. Quantitation was performed using selected ion monitoring of m/z 2364 for α-La. The calibration curve was linear from 0.2 to 10 µg/mL. The intra- and interday precisions were less than 7.6% and the accuracy ranged from 96.4 to 104.5%. The limit of quantification (LOQ) was 0.15 µg/mL and the limit of detection (LOD) was 0.05 µg/mL. This method was then successfully applied to investigate 6 different lactose samples. The application can provide technical preparation for the development of specification of lactose.
乳糖是一种广泛使用的药用辅料，有时不可替代。乳糖生产过程中残留的痕量蛋白质是人体潜在的过敏原。本文描述了一种灵敏且特异的液相色谱 - 质谱法，用于测定乳糖样品中的α - 乳白蛋白（α - La）。色谱分离在Acquity UPLC BEH300 C18柱（2.1×150 mm，1.7 μm）上进行，等度流动相由含0.1%三氟乙酸（TFA）的水和含0.1% TFA的乙腈（80 : 20，v/v）组成。质谱检测通过配备电喷雾电离（ESI）接口且在正离子模式下运行的三重四极杆质谱仪实现。使用m/z 2364对α - La进行选择离子监测进行定量分析。校准曲线在0.2至10 µg/mL范围内呈线性。日内和日间精密度均小于7.6%，准确度范围为96.4%至104.5%。定量限（LOQ）为0.15 µg/mL，检测限（LOD）为0.05 µg/mL。该方法随后成功应用于6种不同乳糖样品的研究。此应用可为乳糖质量标准的制定提供技术准备。
