[Establishment and verification of quality evaluation method of Jizhi Syrup based on quantitative analysis of multi-components by single marker].

A quantitative analysis of multi-components by single marker(QAMS) method was established for the simultaneous determination of ephedrine hydrochloride, protocatechuic acid, 5-caffeoylquinic acid, 4-hydroxybenzoic acid, naringin, neohesperidin, glycyrrhizic acid, and praeruptorin A in Jizhi Syrup by high performance liquid chromatography(HPLC) with ultraviolet multi-wavelength detection system, and its feasibility in quality evaluation of Jizhi syrup was verified. With naringin as the internal reference substance, the relative correction factors and chromatographic peak localization methods of other seven components were respectively established at 210, 254, 280, and 320 nm. The method reproducibility was validated, and the result of QAMS were compared with those obtained by the external standard method(ESM) to verify the accuracy and feasibility of the method. The relative correction factors of ephedrine hydrochloride, protocatechuic acid, 5-caffeoylquinic acid, 4-hydroxybenzoic acid, neohesperidin, glycyrrhizic acid, and praeruptorin A with naringin as reference were 0.846, 0.582, 0.608, 0.293, 0.913, 2.207, and 0.940, respectively, which presented excellent reproducibility under different experimental conditions. Furthermore, QAMS and ESM showed no significant difference in the results for 15 batches of samples. Except protocatechuic acid and 5-caffeoylquinic acid, other six compounds were the exclusive components of single medicinal materials. In addition, glycyrrhizic acid and praeruptorin A were identified in the Jizhi Syrup for the first time, filling up the blank of no component detected in Glycyrrhizae Radix et Rhizoma and Peucedani Radix. The method established in this study is convenient, efficient, specific, accurate, and reliable, which can comprehensively and effectively evaluate the quality of Jizhi Syrup to ensure the safety and efficacy of this drug in clinical application.

Study on Chinese patent medicine based on major component analysis and quality control evaluation: A case study of Jizhi Syrup.

Jizhi Syrup (JZS) is a popular Chinese patent medicine (CPM) for the treatment of respiratory diseases in clinical practice, especially acute or chronic bronchitis. JZS is a complex formula composed of 8 kinds of herbs and lack of comprehensive researches on chemical components. To further define its components, ultra-performance liquid chromatography-quadrupole-time of flight-mass spectrometry (UPLC-Q-TOF-MS) and headspace-solid phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS) were utilized to identify and classify the chemical components of JZS. A total of 178 chemical compounds encompassing the 8 herbs of JZS were identified and the chemical components were comprehensively explicit. It made up for the gap that volatile components were not studied in the previous study. Based on this, a new method for the quality control of JZS based on its characteristic components was established by fingerprints, multi-component quantitative analysis and quantity transfer of JZS. A dual-wavelength high-performance liquid chromatography (HPLC) fingerprints were established at 210 nm and 260 nm. Four volatile components (linalool, bornyl acetate, 2-undecanone and α-terpineol) and eight nonvolatile components (ephedrine hydrochloride, protocatechuic acid, 5-caffeoylquinic acid, 4-hydroxybenzoic acid, naringin, neohesperidin, glycyrrhizic acid and praeruptorin A) were quantitated by HS-SPME-GC-MS and HPLC-diode array detection (DAD). Meanwhile, six exclusive nonvolatile components were studied for the quantity transfer of Herbs-Intermediate-CPM and all the transfer rates were between 55.23% and 89.20%. This study is the first comprehensive study of the major components in JZS, and its results can be useful to standardize the quality control and provide a valuable reference for other CPMs.

Study on HPTLC identification of one-plate multi-drug and HPLC content determination method for Jizhi syrup / 中国药房

OBJECTIVE To optimize the existing t hin layer chromatography （TLC）identification and content determination methods of Jizhi syrup. METHODS High performance thin-layer chromatography （HPTLC）was used to identify five medicinal materials in Jizhi syrup ，such as Ilex chinensis ，Houttuynia cordata ，Peucedanum praeruptorum ，Citrus aurantium ，Glycyrrhiza uralensis. High performance liquid chromatography （HPLC）was used to determine the contents of procatechuic acid ，ephedrine hydrochloride and naringin in Jizhi syrup. RESULTS HPTLC results showed that the identification spots of pedunculoside ， praeruptorin A ，naringin，and liquiritin were clearly displayed ，and the retention factors were in the range of 0.2 to 0.8. After validation，the method had been proved to be strongly specific ，robust and repeatable. HPLC results showed that the linear ranges of protocatechuic acid ，ephedrine hydrochloride and naringin were 4.32-431.67，1.14-114.17 and 7.02-702.33 μg/mL（all r＞ 0.996），respectively. The average recoveries were 100.61％，100.40％ and 99.22％，and RSDs were all less than 2.00％. RSDs of precision（n＝6），stability（24 h，n＝7）and repeatability （n＝6）were all less than 2.00％. The average contents of the three components in 10 batches were 623.3，152.1，1 213.9 μg/mL（RSD＜10.00％），respectively. CONCLUSIONS In this study ， HPTLC method of one-plate multi-drug is established for the identification of Jizhi syrup. One sample pretreatment method and two TLC conditions are used to realize the rapid identification of five kinds of medicinal materials. An HPLC method is established to determine the content of Jizhi syrup ，which realizes the fast quantification of three active components in Jizhi syrup ，and can be used to optimize the identification and content determination items in the existing legal quality standards of Jizhi syrup.