陈皮配方颗粒的质量标准提高研究
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摘要
目的:完善和提高陈皮配方颗粒的质量标准。方法:以4个不同厂家的13批陈皮配方颗粒为试验样品,按2015年版《中国药典》(四部)薄层色谱法(TLC)对样品中橙皮苷和川陈皮素进行定性鉴别;采用超高效液相色谱法(UPLC)对样品中柚皮苷、橙皮苷、橙皮素、川陈皮素和桔皮素进行定量分析[色谱柱为Waters Acquity UPLC BEH C18;流动相为乙腈-0.2%磷酸水溶液,梯度洗脱;检测波长为283 nm;进样量为3μL]。结果:TLC结果显示,在供试品色谱中,与对照品色谱相应位置上均显相同颜色的斑点。UPLC结果显示,柚皮苷、橙皮苷、橙皮素、川陈皮素和桔皮素检测质量浓度的线性范围分别为0.64～6.44、15.78～157.80、0.17～1.66、2.08～20.85和2.04～20.43μg/mL(r均≥0.999 2),检测限分别为0.03、0.33、0.10、0.20和0.06μg/mL,定量限分别为0.07、1.34、0.20、0.60和0.22μg/mL,平均加样回收率分别为99.4%、99.6%、99.7%、99.7%和99.7%(n=9),精密度(n=6)、稳定性(n=7)、重复性(n=6)试验的RSD均≤2.03%。仅在1个厂家的3批样品中检测出了柚皮苷(含量范围为0.067 3～0.069 6 mg/g),而其余4个成分在13批样品中均有检测到,含量范围分别为0.646 5～1.728 0、0.102 6～0.290 5、0.023 1～0.689 8、0.018 2～0.2707 mg/g。结论:本研究通过定性、定量方法完善了陈皮配方颗粒的质量标准,并初步限定了其中橙皮苷、橙皮素、川陈皮素和桔皮素的含量分别不低于0.60、0.10、0.02和0.01 mg/g。
OBJECTIVE:To optimize and improve the quality standard for Citrus reticulata formula granules. METHODS:Totally 13 batches of C. Reticulata formula granules from 4 different manufacturers were used as trial samples,and qualitative identification of hesperidin and nobiletin in the samples were carried out by TLC according to the method of 2015 edition of Chinese Pharmacopoeia(part Ⅳ). The quantitative analysis of naringin,hesperidin,hesperetin,nobiletin and tangeretin in C.reticulatae formula granules were conducted by UPLC[The determination was performed on Waters Acquity UPLC BEH C18 column with mobile phase consisted of acetonitrile-0.2% phosphoric acid aqueous solution(gradient elution). The detection wavelength was set at 283 nm,and sample size was 3 μL]. RESULTS:The results of TLC showed that in the chromatograms of samples,same color spots were shown in the corresponding positions of the chromatogram of reference substance. The results of UPLC showed,that the linear range of naringin,hesperidin,hesperetin,nobiletin and tangeretin were 0.64-6.44,15.78-157.80,0.17-1.66,2.08-20.85 and 2.04-20.43 μg/mL,respectively(all r≥0.999 2);the limits of detection were 0.03,0.33,0.10,0.20 and 0.06 μg/mL;the limits of quantitation were 0.07,1.34,0.20,0.60 and 0.22 μg/mL. The average recoveries were 99.4%,99.6%,99.7%,99.7% and 99.7%(n=9);RSDs of precision(n=6),stability(n=7)and reproducibility(n=6)tests were all≤2.03%;naringin was detected in only 3 batches of samples from one manufacturer(the content ranged from 0.067 3 to 0.069.6 mg/g),while the other 4 components were detected in 13 batches of samples(the contents of them ranged 0.646 5-1.728 0, 0.102 6-0.290 5,0.0231-0.689 8,0.018 2-0.270 7 mg/g). CONCLUSIONS:In this study,the quality standard of C. reticulata formula granules was improved by qualitative and quantitative methods,and the contents of hesperidin,hesperetin,nobiletin and tangeretin were not less than 0.60,0.10,0.02 and 0.01 mg/g,respectively.
OBJECTIVE:To optimize and improve the quality standard for Citrus reticulata formula granules. METHODS:Totally 13 batches of C. Reticulata formula granules from 4 different manufacturers were used as trial samples,and qualitative identification of hesperidin and nobiletin in the samples were carried out by TLC according to the method of 2015 edition of Chinese Pharmacopoeia(part Ⅳ). The quantitative analysis of naringin,hesperidin,hesperetin,nobiletin and tangeretin in C.reticulatae formula granules were conducted by UPLC[The determination was performed on Waters Acquity UPLC BEH C18 column with mobile phase consisted of acetonitrile-0.2% phosphoric acid aqueous solution(gradient elution). The detection wavelength was set at 283 nm,and sample size was 3 μL]. RESULTS:The results of TLC showed that in the chromatograms of samples,same color spots were shown in the corresponding positions of the chromatogram of reference substance. The results of UPLC showed,that the linear range of naringin,hesperidin,hesperetin,nobiletin and tangeretin were 0.64-6.44,15.78-157.80,0.17-1.66,2.08-20.85 and 2.04-20.43 μg/mL,respectively(all r≥0.999 2);the limits of detection were 0.03,0.33,0.10,0.20 and 0.06 μg/mL;the limits of quantitation were 0.07,1.34,0.20,0.60 and 0.22 μg/mL. The average recoveries were 99.4%,99.6%,99.7%,99.7% and 99.7%(n=9);RSDs of precision(n=6),stability(n=7)and reproducibility(n=6)tests were all≤2.03%;naringin was detected in only 3 batches of samples from one manufacturer(the content ranged from 0.067 3 to 0.069.6 mg/g),while the other 4 components were detected in 13 batches of samples(the contents of them ranged 0.646 5-1.728 0, 0.102 6-0.290 5,0.0231-0.689 8,0.018 2-0.270 7 mg/g). CONCLUSIONS:In this study,the quality standard of C. reticulata formula granules was improved by qualitative and quantitative methods,and the contents of hesperidin,hesperetin,nobiletin and tangeretin were not less than 0.60,0.10,0.02 and 0.01 mg/g,respectively.
引文
[1]国家药典委员会.中华人民共和国药典:一部[S]. 2015年版.北京:中国医药科技出版社,2015:191.
[2]李晓芳,张健康,王慧鸾,等.陈皮的研究进展[J].江西中医药,2014,11(24):154-156.
[3]李柯柯,任顺成.陈皮中黄酮类化合物的研究进展[J].食品研究与开发,2017,38(17):221-224.
[4]俞静静,苏洁,吕圭源.陈皮抗心脑血管疾病相关药理研究进展[J].中草药,2016,47(17):3127-3132.
[5]樊如强,夏立武,李进飞.陈皮配方颗粒一步制粒工艺研究[J].时珍国医国药,2017,28(9):2149-2151.
[6]吴玢,付静,张翠.一种陈皮配方颗粒及其制备方法和质量控制方法:中国,CN200710175354.X[P]. 2009-04-01.
[7]何军,朱旭江,杨平荣,等.中药配方颗粒的现状与发展新思路[J].中草药,2018,49(20):4717-4725.
[8]黄华轼. HPLC法测定陈皮配方颗粒中橙皮苷的含量[J].江西中医学院学报,2004,16(2):66.
[9]罗文汇,李养学,孙冬梅,等.陈皮配方颗粒质量标准研究[J].中国药业,2011,20(2):32-33.
[10]李文东,梅雪,赵玉玺,等.高效液相色谱法同时测定陈皮配方颗粒中3种成分的含量[J].安徽医药,2018,22(9):1670-1673.
[11]国家药典委员会.中华人民共和国药典:四部[S]. 2015年版.北京:中国医药科技出版社,2015:57-59.
[12]高俊丽,邵艳华,李倩,等.广陈皮及其近缘种药用植物的HPTLC研究[J].中国现代中药,2015,17(10):1020-1025.
[13]周芳,郑国栋,蒋林,等.薄层扫描法同时测定广陈皮中三种黄酮化合物的含量[J].中药材,2009,32(6):911-913.
[14]冉玥,焦必宁,赵其阳,等.超高效液相色谱法同时测定柑橘中11种类黄酮物质[J].食品科学,2013,34(4):168-172.
[15]钟永翠,巩珺,徐家能,等.基于3种黄酮类化合物含量比值鉴别广陈皮道地性[J].药物分析杂志,2017,37(1):20-29.
[16]张菊华,李志坚,单杨,等.柑桔鲜果皮中类黄酮含量比较与分析[J].中国食品学报,2015,15(5):233-240.
[17]骆骄阳,周文菊,李坤伦,等.不同储藏环境和包装形式对陈皮质量的影响[J].中国中药杂志,2018,43(5):985-992.
[18]李积东,黄起壬.柚皮苷的分离提取及药理作用研究进展[J].北方药学,2014,11(7):67-68.
[19]游琼,吴铿.柚皮苷的心血管药理作用[J].广东医学,2010,31(22):3006-3007.
[20]张恒,饶坤林,向韩.橙皮苷药理活性研究进展[J].中南药学,2016,14(10):1097-1100.
[21]李丽,任周新,赵鹏,等.橙皮苷及橙皮素抗肿瘤药理活性研究进展[J].中医学报,2018,12(33):2304-2308.
[22]巢同磊,王欠欠.橙皮素及其衍生物的药理作用研究进展[J].中草药,2018,49(14):3446-3451.
[23]叶喜德,黄兆胜,骆利平,等.川陈皮素研究概括[J].江西中医学院学报,2013,25(3):42-45.
[24]于宏伟,韩卫荣,周二鹏,等.橘皮素的提取及应用研究进展[J].江苏农业科学,2012,40(3):249-252.
[25]孙志欣,张莹.桔皮素对人肝癌HepG2细胞体外增殖和侵袭的影响及机制研究[J].中国药房,2016,27(34):4800-4803.
[2]李晓芳,张健康,王慧鸾,等.陈皮的研究进展[J].江西中医药,2014,11(24):154-156.
[3]李柯柯,任顺成.陈皮中黄酮类化合物的研究进展[J].食品研究与开发,2017,38(17):221-224.
[4]俞静静,苏洁,吕圭源.陈皮抗心脑血管疾病相关药理研究进展[J].中草药,2016,47(17):3127-3132.
[5]樊如强,夏立武,李进飞.陈皮配方颗粒一步制粒工艺研究[J].时珍国医国药,2017,28(9):2149-2151.
[6]吴玢,付静,张翠.一种陈皮配方颗粒及其制备方法和质量控制方法:中国,CN200710175354.X[P]. 2009-04-01.
[7]何军,朱旭江,杨平荣,等.中药配方颗粒的现状与发展新思路[J].中草药,2018,49(20):4717-4725.
[8]黄华轼. HPLC法测定陈皮配方颗粒中橙皮苷的含量[J].江西中医学院学报,2004,16(2):66.
[9]罗文汇,李养学,孙冬梅,等.陈皮配方颗粒质量标准研究[J].中国药业,2011,20(2):32-33.
[10]李文东,梅雪,赵玉玺,等.高效液相色谱法同时测定陈皮配方颗粒中3种成分的含量[J].安徽医药,2018,22(9):1670-1673.
[11]国家药典委员会.中华人民共和国药典:四部[S]. 2015年版.北京:中国医药科技出版社,2015:57-59.
[12]高俊丽,邵艳华,李倩,等.广陈皮及其近缘种药用植物的HPTLC研究[J].中国现代中药,2015,17(10):1020-1025.
[13]周芳,郑国栋,蒋林,等.薄层扫描法同时测定广陈皮中三种黄酮化合物的含量[J].中药材,2009,32(6):911-913.
[14]冉玥,焦必宁,赵其阳,等.超高效液相色谱法同时测定柑橘中11种类黄酮物质[J].食品科学,2013,34(4):168-172.
[15]钟永翠,巩珺,徐家能,等.基于3种黄酮类化合物含量比值鉴别广陈皮道地性[J].药物分析杂志,2017,37(1):20-29.
[16]张菊华,李志坚,单杨,等.柑桔鲜果皮中类黄酮含量比较与分析[J].中国食品学报,2015,15(5):233-240.
[17]骆骄阳,周文菊,李坤伦,等.不同储藏环境和包装形式对陈皮质量的影响[J].中国中药杂志,2018,43(5):985-992.
[18]李积东,黄起壬.柚皮苷的分离提取及药理作用研究进展[J].北方药学,2014,11(7):67-68.
[19]游琼,吴铿.柚皮苷的心血管药理作用[J].广东医学,2010,31(22):3006-3007.
[20]张恒,饶坤林,向韩.橙皮苷药理活性研究进展[J].中南药学,2016,14(10):1097-1100.
[21]李丽,任周新,赵鹏,等.橙皮苷及橙皮素抗肿瘤药理活性研究进展[J].中医学报,2018,12(33):2304-2308.
[22]巢同磊,王欠欠.橙皮素及其衍生物的药理作用研究进展[J].中草药,2018,49(14):3446-3451.
[23]叶喜德,黄兆胜,骆利平,等.川陈皮素研究概括[J].江西中医学院学报,2013,25(3):42-45.
[24]于宏伟,韩卫荣,周二鹏,等.橘皮素的提取及应用研究进展[J].江苏农业科学,2012,40(3):249-252.
[25]孙志欣,张莹.桔皮素对人肝癌HepG2细胞体外增殖和侵袭的影响及机制研究[J].中国药房,2016,27(34):4800-4803.