Department of Chemistry, University of Washington, Seattle, WA 98195, USA.
Clin Chem. 2011 Jan;57(1):128-31. doi: 10.1373/clinchem.2010.149880. Epub 2010 Oct 28.
Treatments are being developed for an increasing number of mucopolysaccharidoses, and early diagnosis is expected to be necessary to maximize the benefits of therapy. Therefore, we developed an assay for N-acetylgalactosamine-6-sulfate sulfatase (GALNS), the enzyme deficient in mucopolysaccharidosis IVA (Morquio A syndrome), that is applicable for clinical diagnosis.
A novel substrate for GALNS was synthesized for a new enzyme activity assay that is based on tandem mass spectrometry and uses dried blood spots (DBSs) as the enzyme source. We optimized the assay conditions, including the substrate concentration, reaction pH, lead formate concentration, incubation time, punch size of the DBS, and mass spectrometer conditions. We also assessed inter- and intraassay variation.
The assay uses either solid-phase or liquid-phase extraction before analysis by mass spectrometry. An evaluation of blood spots from 90 randomly chosen healthy newborns and 9 patients with Morquio A syndrome showed a well-defined interval between their respective enzyme activities. Inter- and intraassay imprecision was <10%.
This tandem mass spectrometry assay requires a minimal number of sample-preparation steps, thus making it easy to implement. The assay has the potential to be adopted for early diagnosis of Morquio A syndrome. We believe this assay could be performed in a multiplex fashion with assays for other lysosomal enzymes.
越来越多的黏多糖贮积症正在开发治疗方法,预计早期诊断对于最大限度地提高治疗效果是必要的。因此,我们开发了一种用于 N-乙酰半乳糖胺-6-硫酸酯酶(GALNS)的检测方法,该酶在黏多糖贮积症 IVA(Morquio A 综合征)中缺乏,适用于临床诊断。
我们合成了一种用于新酶活性测定的新型 GALNS 底物,该测定基于串联质谱法,并使用干血斑(DBS)作为酶源。我们优化了测定条件,包括底物浓度、反应 pH 值、甲酸铅浓度、孵育时间、DBS 的打孔大小和质谱仪条件。我们还评估了批内和批间变异。
该测定在通过质谱分析之前使用固相或液相提取。对 90 名随机选择的健康新生儿和 9 名 Morquio A 综合征患者的血斑进行评估,显示其各自的酶活性之间有明确的间隔。批内和批间精密度均<10%。
这种串联质谱测定需要最少的样品制备步骤,因此易于实施。该测定有可能用于 Morquio A 综合征的早期诊断。我们认为该测定可以与其他溶酶体酶的测定一起以多重方式进行。