Abstract:OBJECTIVE To verify a new reference standard for N-glycyl-L-tyrosine in order to assure the quality of amino acids (15) and dipeptides (2) injection. METHODS UV, HRMS,1H-NMR,13C-NMR and 2D NMR were used to confirm the structure, and the content of the product was calculated by mass balance method, which was also confirmed by titrimetric method. RESULTS The structure of this product was identified and the content of N-glycyl-L-tyrosine was assigned as 88.4%. CONCLUSION According to the physicochemical properties of the compound, were used multiple methods for the qualitative and quatitative analysis to ensure the calibration results of the national reference standard accurately. The first established N-glycyl-L-tyrosine national reference can be efficiently applied for the assay of amino acids (15) and dipeptides (2) injection.
刘博, 任丽萍, 张佟, 黄姗, 范慧红. 首批甘氨酰-L-酪氨酸国家对照品的标定研究[J]. 中国药学杂志, 2020, 55(22): 1890-1894.
LIU Bo, REN Li-ping, ZHANG Tong, HUANG Shan, FAN Hui-hong. Verification of National Reference Standard of N-glycyl-L-tyrosine. Chinese Pharmaceutical Journal, 2020, 55(22): 1890-1894.
ZHU Q, FENG Q Q, XIAO Y, et al. Study on the test method for bacterial endotoxin in compound amino acids(15AA)and dipeptide(2) injection [J]. J China Pharm(中国药房), 2016, 27(33):4742- 4744.
[2]
WANG J, YANG H, PAN X, et al. Determination of three impurities in compound amino acids (15) and dipeptides (2) injections by HPLC[J]. China Pharm(中国药师), 2013, 16 (1):87-89.
[3]
XIE X, CHU Y, BAI X, et al. Clinical analysis of compound amino acid (15) and dipeptides (2) injection[J]. J Pharm Parct(药学实践杂志), 2014, 32 (5):374-375.
FENG Y, WANG C, TIAN Y, et al. Establishment of national reference standard of fluconazole impurity H[J]. Chin Pharm J(中国药学杂志),2018, 53(17):1516-1522.
[6]
ZUO N, CHEN H, NAN N. Establishment of national reference panel for methamphetamine kits[J]. Chin Pharm J(中国药学杂志),2016, 51 (15):1330-1335.
[7]
LIAO H, REN X, LI Y. Devement of the first batch national reference substance for tyroserleutide[J]. Chin Pharm Aff(中国药事), 2013, 27(19):402-407.
[8]
LENG X, SHI S, LI Y, et al. Quantitative determination of gluconic acid in oral solution NMR[J]. Chin Reagent(化学试剂),2019, 41(6):598-602.
[9]
GAO W, SUN L, WANG Q H. Quantitative determination of ligustilide by 1H-nuclear magnetic resonance spectroscopy[J]. Chin Pharm J(中国药学杂志), 2017, 52(22):2042-2046.
[10]
ZHANG C Y, NING B M, HE L. Application of the quantity nuclear magnetic method in the calibration of the chemical reference substances[J]. Chin J Pharm Anal (药物分析杂志), 2019, 33(5):919-924.
[11]
XIA Z X, FENG Y, ZHANG Y, et al. Establishment of a quantitative 1H-NMR method for reference standards of trazodone hydrochloride impurity[J]. Chin J Pharm Anal (药物分析杂志), 2019, 33(5):925-929.
[12]
LIU Y, WEI N, YUE R, et al. 19F qNMR Application of novel 19F quantitative NMR(19F-qNMR)in assay of droperidol[J]. Chin J New Drugs(中国新药杂志), 2014, 23(16):1960-1962.
[13]
GUIDO F P. QNMR-a versatile concept for the validation of natural product reference compounds[J]. Phytochem Anal, 2001, 12(1):28-42.
[14]
SIDNEI M, FELIPE G C, CAROLINA D R O, et al. qNMR: an applicable method for the determination of dimethyltryptamine in ayahuasca, a psychoactive plant preparation[J]. Phytochemistry Lett, 2010, 3(2):79-83.
[15]
World Health Organization. WHO Technical ReportsSeries No.943 (Part A), General Guidelines for the Establishment, Maintenance and Distribution of Chemical Reference Substance[S]. 2007:65-71.