Wenfan Nie, Ying Wang, Jinhui Du, Wei Mi, Kexin Qi, Zhonglian Zhang, Zhifei Fu, Lifeng Han
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The offline 2D-LC system, consisting of an XAmide column and an HSS T<sub>3</sub> column, exhibited an orthogonality of 0.61 and a theoretical peak capacity of 7038. As a result, a total of 153 compounds were identified. Subsequently, an online two-dimensional liquid chromatography/quadrupole-time-of-flight MS (online 2D-LC/Q-TOF–MS) method was developed. The online system, integrating a Poroshell 120 HILIC-Z column (first dimension) and a Poroshell 120 Aq-C18 column (second dimension), exhibited an orthogonality of 0.58 and a better peak capacity of 8675. The component screening capability was preliminarily evaluated and compared with the offline 2D-LC–MS method. A total of 177 compounds were detected, and after removing duplicates identified in the offline system, 263 compounds were ultimately characterized. Finally, a co-condition fingerprint analysis for four single herbs of SJMS was performed, identifying seven bioactive compounds (chlorogenic acid, liquiritin, cynaroside, nodakenin, linarin, glycyrrhizic acid, and aurantio-obtusin) as quality markers of SJMS. An adjusted multiple reaction monitoring (MRM<sup>ad</sup>) method based on UPLC-QQQ-MS was established for the quantitative analysis of these markers in 15 batches of SJMS. This study represents comprehensive multi-component characterization, identification, and quality control of SJMS for the first time, providing a scientific basis for its quality control.</p><h3>Graphical Abstract</h3>\n<div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":"417 23","pages":"5221 - 5237"},"PeriodicalIF":3.8000,"publicationDate":"2025-08-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Systematic quality control of Shi Jue Ming San by two-dimensional liquid chromatography/mass spectrometry and adjusted multiple reaction monitoring of quality markers\",\"authors\":\"Wenfan Nie, Ying Wang, Jinhui Du, Wei Mi, Kexin Qi, Zhonglian Zhang, Zhifei Fu, Lifeng Han\",\"doi\":\"10.1007/s00216-025-06041-5\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div><p>Shi Jue Ming San (SJMS) is a traditional Chinese medicine formula, which is primarily used in clinical practice for treating hypertension and eye diseases. However, due to the complex composition of SJMS, studies on its quality control and chemical constituents remain limited. This study aims to establish a systematic quality control method on SJMS through qualitative and quantitative analyses using chromatography-mass spectrometry. Firstly, an offline two-dimensional liquid chromatography/quadrupole-Orbitrap-MS method (offline 2D-LC/Q-Orbitrap-MS) was established for multi-component characterization. The offline 2D-LC system, consisting of an XAmide column and an HSS T<sub>3</sub> column, exhibited an orthogonality of 0.61 and a theoretical peak capacity of 7038. As a result, a total of 153 compounds were identified. Subsequently, an online two-dimensional liquid chromatography/quadrupole-time-of-flight MS (online 2D-LC/Q-TOF–MS) method was developed. The online system, integrating a Poroshell 120 HILIC-Z column (first dimension) and a Poroshell 120 Aq-C18 column (second dimension), exhibited an orthogonality of 0.58 and a better peak capacity of 8675. The component screening capability was preliminarily evaluated and compared with the offline 2D-LC–MS method. A total of 177 compounds were detected, and after removing duplicates identified in the offline system, 263 compounds were ultimately characterized. Finally, a co-condition fingerprint analysis for four single herbs of SJMS was performed, identifying seven bioactive compounds (chlorogenic acid, liquiritin, cynaroside, nodakenin, linarin, glycyrrhizic acid, and aurantio-obtusin) as quality markers of SJMS. An adjusted multiple reaction monitoring (MRM<sup>ad</sup>) method based on UPLC-QQQ-MS was established for the quantitative analysis of these markers in 15 batches of SJMS. 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Systematic quality control of Shi Jue Ming San by two-dimensional liquid chromatography/mass spectrometry and adjusted multiple reaction monitoring of quality markers
Shi Jue Ming San (SJMS) is a traditional Chinese medicine formula, which is primarily used in clinical practice for treating hypertension and eye diseases. However, due to the complex composition of SJMS, studies on its quality control and chemical constituents remain limited. This study aims to establish a systematic quality control method on SJMS through qualitative and quantitative analyses using chromatography-mass spectrometry. Firstly, an offline two-dimensional liquid chromatography/quadrupole-Orbitrap-MS method (offline 2D-LC/Q-Orbitrap-MS) was established for multi-component characterization. The offline 2D-LC system, consisting of an XAmide column and an HSS T3 column, exhibited an orthogonality of 0.61 and a theoretical peak capacity of 7038. As a result, a total of 153 compounds were identified. Subsequently, an online two-dimensional liquid chromatography/quadrupole-time-of-flight MS (online 2D-LC/Q-TOF–MS) method was developed. The online system, integrating a Poroshell 120 HILIC-Z column (first dimension) and a Poroshell 120 Aq-C18 column (second dimension), exhibited an orthogonality of 0.58 and a better peak capacity of 8675. The component screening capability was preliminarily evaluated and compared with the offline 2D-LC–MS method. A total of 177 compounds were detected, and after removing duplicates identified in the offline system, 263 compounds were ultimately characterized. Finally, a co-condition fingerprint analysis for four single herbs of SJMS was performed, identifying seven bioactive compounds (chlorogenic acid, liquiritin, cynaroside, nodakenin, linarin, glycyrrhizic acid, and aurantio-obtusin) as quality markers of SJMS. An adjusted multiple reaction monitoring (MRMad) method based on UPLC-QQQ-MS was established for the quantitative analysis of these markers in 15 batches of SJMS. This study represents comprehensive multi-component characterization, identification, and quality control of SJMS for the first time, providing a scientific basis for its quality control.
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