{"title":"固相萃取-串联质谱联用快速测定尿中儿茶酚胺和总肾上腺素","authors":"Yuhan Li, Guangming Huang","doi":"10.1002/rcm.10077","DOIUrl":null,"url":null,"abstract":"<div>\n \n \n <section>\n \n <h3> Rationale</h3>\n \n <p>The measurement of urinary catecholamines and total metanephrines serves as one of the primary tests in the diagnosis of pheochromocytoma and paraganglioma (PPGL). The widely adopted liquid chromatography–tandem mass spectrometry (LC–MS/MS) method, however, typically necessitates sample pretreatments and chromatographic separation prior to MS, resulting in challenges for facile and rapid screening of targets from complex matrices. Therefore, it is crucial to develop an analytical method that can rapidly and efficiently detect urinary catecholamines and total metanephrines.</p>\n </section>\n \n <section>\n \n <h3> Methods</h3>\n \n <p>A rapid and time-efficient procedure using solid-phase extraction (SPE) combined with pulsed direct current electrospray ionization tandem mass spectrometry (pulsed-dc-ESI-MS/MS) was validated for the specific and quantitative analysis of six urinary catecholamines and metanephrines. The SPE protocol was specifically optimized to enable direct analysis of the eluate obtained from SPE using MS/MS. All six compounds could be detected in a single complete operation.</p>\n </section>\n \n <section>\n \n <h3> Results</h3>\n \n <p>The method was evaluated by the determination of catecholamines and metanephrines (dopamine, epinephrine, norepinephrine, normetanephrine, metanephrine, and 3-methoxytyramine) in artificial urine samples and raw urine samples. Under the optimized experimental conditions, the limits of detection for these six analytes were in the range of 0.02–68.37 nM L<sup>−1</sup>, using dopamine-d4 (DA-d4) and metanephrines-d3 (MN-d3) as internal standards, respectively, which achieved the detection requirements for the clinical diagnosis of PPGL.</p>\n </section>\n \n <section>\n \n <h3> Conclusions</h3>\n \n <p>SPE coupled with pulsed-dc-ESI-MS/MS demonstrated improved efficiency compared to existing methods, which successfully enabled the rapid screening of urinary catecholamines and total metanephrines. Therefore, we believe that this method could be potentially useful in the clinical screening of PPGL and suitable for the direct analysis of urine.</p>\n </section>\n </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 17","pages":""},"PeriodicalIF":1.7000,"publicationDate":"2025-06-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Solid-Phase Extraction Coupled to Tandem Mass Spectrometry for Rapid Quantitation of Urinary Catecholamines and Total Metanephrines\",\"authors\":\"Yuhan Li, Guangming Huang\",\"doi\":\"10.1002/rcm.10077\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div>\\n \\n \\n <section>\\n \\n <h3> Rationale</h3>\\n \\n <p>The measurement of urinary catecholamines and total metanephrines serves as one of the primary tests in the diagnosis of pheochromocytoma and paraganglioma (PPGL). The widely adopted liquid chromatography–tandem mass spectrometry (LC–MS/MS) method, however, typically necessitates sample pretreatments and chromatographic separation prior to MS, resulting in challenges for facile and rapid screening of targets from complex matrices. Therefore, it is crucial to develop an analytical method that can rapidly and efficiently detect urinary catecholamines and total metanephrines.</p>\\n </section>\\n \\n <section>\\n \\n <h3> Methods</h3>\\n \\n <p>A rapid and time-efficient procedure using solid-phase extraction (SPE) combined with pulsed direct current electrospray ionization tandem mass spectrometry (pulsed-dc-ESI-MS/MS) was validated for the specific and quantitative analysis of six urinary catecholamines and metanephrines. The SPE protocol was specifically optimized to enable direct analysis of the eluate obtained from SPE using MS/MS. All six compounds could be detected in a single complete operation.</p>\\n </section>\\n \\n <section>\\n \\n <h3> Results</h3>\\n \\n <p>The method was evaluated by the determination of catecholamines and metanephrines (dopamine, epinephrine, norepinephrine, normetanephrine, metanephrine, and 3-methoxytyramine) in artificial urine samples and raw urine samples. Under the optimized experimental conditions, the limits of detection for these six analytes were in the range of 0.02–68.37 nM L<sup>−1</sup>, using dopamine-d4 (DA-d4) and metanephrines-d3 (MN-d3) as internal standards, respectively, which achieved the detection requirements for the clinical diagnosis of PPGL.</p>\\n </section>\\n \\n <section>\\n \\n <h3> Conclusions</h3>\\n \\n <p>SPE coupled with pulsed-dc-ESI-MS/MS demonstrated improved efficiency compared to existing methods, which successfully enabled the rapid screening of urinary catecholamines and total metanephrines. 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引用次数: 0
摘要
尿儿茶酚胺和总肾上腺素的测定是诊断嗜铬细胞瘤和副神经节瘤（PPGL）的主要检查之一。然而，广泛采用的液相色谱-串联质谱（LC-MS /MS）方法通常需要在质谱之前进行样品预处理和色谱分离，这给从复杂基质中方便快速筛选目标带来了挑战。因此，开发一种能够快速有效检测尿儿茶酚胺和总肾上腺素的分析方法至关重要。方法采用固相萃取（SPE）联合脉冲直流电喷雾串联质谱（pulsed-dc- esi -MS/MS）技术，对6种尿中儿茶酚胺和肾上腺素进行特异性定量分析。对固相萃取方案进行了优化，使固相萃取得到的洗脱液可以用MS/MS直接分析。所有六种化合物都可以在一次完整的操作中检测到。结果通过测定人工尿样和原始尿样中儿茶酚胺和肾上腺素（多巴胺、肾上腺素、去甲肾上腺素、去甲肾上腺素、去甲肾上腺素、3-甲氧基酪胺）的含量，对该方法进行了评价。在优化的实验条件下，以多巴胺-d4 （DA-d4）和肾上腺素-d3 （MN-d3）为内标物，6种分析物的检出限在0.02 ~ 68.37 nM L−1范围内，达到PPGL临床诊断的检测要求。结论与现有方法相比，SPE联合脉冲dc- esi -MS/MS具有更高的效率，能够快速筛选尿中儿茶酚胺和总肾上腺素。因此，我们认为该方法可用于PPGL的临床筛查，适合于尿液的直接分析。
Solid-Phase Extraction Coupled to Tandem Mass Spectrometry for Rapid Quantitation of Urinary Catecholamines and Total Metanephrines
Rationale
The measurement of urinary catecholamines and total metanephrines serves as one of the primary tests in the diagnosis of pheochromocytoma and paraganglioma (PPGL). The widely adopted liquid chromatography–tandem mass spectrometry (LC–MS/MS) method, however, typically necessitates sample pretreatments and chromatographic separation prior to MS, resulting in challenges for facile and rapid screening of targets from complex matrices. Therefore, it is crucial to develop an analytical method that can rapidly and efficiently detect urinary catecholamines and total metanephrines.
Methods
A rapid and time-efficient procedure using solid-phase extraction (SPE) combined with pulsed direct current electrospray ionization tandem mass spectrometry (pulsed-dc-ESI-MS/MS) was validated for the specific and quantitative analysis of six urinary catecholamines and metanephrines. The SPE protocol was specifically optimized to enable direct analysis of the eluate obtained from SPE using MS/MS. All six compounds could be detected in a single complete operation.
Results
The method was evaluated by the determination of catecholamines and metanephrines (dopamine, epinephrine, norepinephrine, normetanephrine, metanephrine, and 3-methoxytyramine) in artificial urine samples and raw urine samples. Under the optimized experimental conditions, the limits of detection for these six analytes were in the range of 0.02–68.37 nM L−1, using dopamine-d4 (DA-d4) and metanephrines-d3 (MN-d3) as internal standards, respectively, which achieved the detection requirements for the clinical diagnosis of PPGL.
Conclusions
SPE coupled with pulsed-dc-ESI-MS/MS demonstrated improved efficiency compared to existing methods, which successfully enabled the rapid screening of urinary catecholamines and total metanephrines. Therefore, we believe that this method could be potentially useful in the clinical screening of PPGL and suitable for the direct analysis of urine.
期刊介绍：
Rapid Communications in Mass Spectrometry is a journal whose aim is the rapid publication of original research results and ideas on all aspects of the science of gas-phase ions; it covers all the associated scientific disciplines. There is no formal limit on paper length ("rapid" is not synonymous with "brief"), but papers should be of a length that is commensurate with the importance and complexity of the results being reported. Contributions may be theoretical or practical in nature; they may deal with methods, techniques and applications, or with the interpretation of results; they may cover any area in science that depends directly on measurements made upon gaseous ions or that is associated with such measurements.
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