HPLC-DAD法同时测定小儿退热合剂中多指标成分含量
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摘要
目的:建立同时测定小儿退热合剂中8个成分的方法。方法:采用DIKMA Platisil ODS色谱柱(250mm×4.6 mm,5μm),柱温35℃,流动相为乙腈-0.1%磷酸水溶液,采用梯度洗脱,变换波长检测,分别为240 nm(京尼平苷酸、京尼平龙胆双糖苷、京尼平苷)、274 nm(绿原酸、黄芩苷、丹皮酚)和210 nm(连翘苷、柴胡皂苷A),流速为1 mL·min~(-1)。结果:京尼平苷酸、京尼平龙胆双糖苷、京尼平苷、绿原酸、黄芩苷、丹皮酚、连翘苷、柴胡皂苷A的线性范围分别为1.17～9.36 ng·mL~(-1)(r=0.999 5),1.98～15.84 ng·mL~(-1)(r=0.999 7),8.00-64.00 ng·mL~(-1)(r=0.999 9),1.64～13.12 ng·mL~(-1)(r=0.999 8),7.00～56.00 ng·mL~(-1)(r=0.999 9),1.096～8.768 ng·mL~(-1)(r=0.999 9),0.56～4.48 ng·mL~(-1)(r=0.999 9),6.20～49.60 ng·mL~(-1)(r=0.999 8),平均回收率在95.2～103.0%之间。3批样品中上述8个成分的含量测定结果分别为0.124 4～0.125 2、0.172 4～0.172 9、1.331 4～1.331 9、0.129 2～0.130 3、1.543 3～1.544 1、0.107 3～0.107 6、0.304～0.308、0.373 0～0.374 5mg·mL~(-1)。结论:该法检测简便,稳定,可靠,可用于小儿退热合剂质量控制。
Objective:To establish a method for simultaneous determination of eight components in Xiaoer Tuire mixture.Methods:The separation was performed on a DIKMA Platisil ODS column(250 mm×4. 6 mm,5 μm),column temperature was 35℃,acetonitriles and 0.1% H_3PO_4 aqueous solution was used as mobile phase for gradient elution.Detection wavelengths were 240 nm for geniposidic acid,genipin 1-gentiobioside,geniposide,274 nm for chlorogenic acid,baicalin,paeonol and 210 nm for phillyroside,saikosaponin A,respectively. The flow rate was 1 mL·min~(-1).Results:Linear ranges of geniposidic acid,genipin 1-gentiobioside,geniposide,chlorogenic acid,baicalin,paeonol,phillyroside,saikosaponin A concentrations were 1.17-9.36 ng·mL~(-1)(r=0.999 5),1.98-15.84 ng·mL~(-1)(r=0.999 7),8.00-64.00 ng·mL~(-1)(r=0.999 9),1.64-13.12 ng·mL~(-1)(r=0.999 8),7.00-56.00 ng·mL~(-1)(r=0.999 9),1.096-8.768 ng·mL~(-1)(r=0.999 9),0.56-4.48 ng·mL~(-1)(r=0.999 9),6.20-49.60 ng·mL~(-1)(r=0.999 8),respectively. Their average recovery rates fell between 95.21% and 103.02%. The contents of the eight components in 3 batches of samples were 0.124 4-0.125 2,0.172 4-0.172 9,1.331 4-1.331 9,0.1292-0.130 3,1.543 3-1.544 1,0.107 3-0.107 6,0.304-0.308,0.373 0-0.374 5 mg·mL~(-1). Conclusion:The method established is simple,stable,reliable and can be used as an effective method for quality control of Xiaoer Tuire mixture.
Objective:To establish a method for simultaneous determination of eight components in Xiaoer Tuire mixture.Methods:The separation was performed on a DIKMA Platisil ODS column(250 mm×4. 6 mm,5 μm),column temperature was 35℃,acetonitriles and 0.1% H_3PO_4 aqueous solution was used as mobile phase for gradient elution.Detection wavelengths were 240 nm for geniposidic acid,genipin 1-gentiobioside,geniposide,274 nm for chlorogenic acid,baicalin,paeonol and 210 nm for phillyroside,saikosaponin A,respectively. The flow rate was 1 mL·min~(-1).Results:Linear ranges of geniposidic acid,genipin 1-gentiobioside,geniposide,chlorogenic acid,baicalin,paeonol,phillyroside,saikosaponin A concentrations were 1.17-9.36 ng·mL~(-1)(r=0.999 5),1.98-15.84 ng·mL~(-1)(r=0.999 7),8.00-64.00 ng·mL~(-1)(r=0.999 9),1.64-13.12 ng·mL~(-1)(r=0.999 8),7.00-56.00 ng·mL~(-1)(r=0.999 9),1.096-8.768 ng·mL~(-1)(r=0.999 9),0.56-4.48 ng·mL~(-1)(r=0.999 9),6.20-49.60 ng·mL~(-1)(r=0.999 8),respectively. Their average recovery rates fell between 95.21% and 103.02%. The contents of the eight components in 3 batches of samples were 0.124 4-0.125 2,0.172 4-0.172 9,1.331 4-1.331 9,0.1292-0.130 3,1.543 3-1.544 1,0.107 3-0.107 6,0.304-0.308,0.373 0-0.374 5 mg·mL~(-1). Conclusion:The method established is simple,stable,reliable and can be used as an effective method for quality control of Xiaoer Tuire mixture.
引文
[1]中华人民共和国药典2015年版.一部[S].2015:544ChP 2015.VolⅠ[S].2015:544
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[5]聂聪珍.高效液相色谱法测定小儿退热合剂中栀子苷的含量[J].中国医药指南,2013,11(14):486NIE CZ.Determination of geniposide in Xiaoer Tuire mixture by HPLC[J].Guide China Med,2013,11(14):486
[6]雷志英,龚建平,彭静.高效液相色谱法同时测定小儿退热口服液中黄芩苷和连翘苷的含量[J].中南药学,2010,8(5):359LEI ZY,GONG JP,PENG J.Determination of baicalin and phillyrin in Xiaoer tuire oral liquid by HPLC[J].Cent South Pharm,2010,8(5):359
[7]张小妹.10批次小儿退烧口服液不符规定被召回[J].广西质量监督导报,2016(1):21ZHANG XM.The tenth batch of Xiaoer Tuire Oral solution is recalled[J].Guangxi Qual Supervis Guide Period,2016(1):21
[8]张琳,汪轩,邢婧,等.HPLC-DAD同时测定左归丸药液中没食子酸、原儿茶酸、绿原酸、马钱苷、阿魏酸含量[J].药物分析杂志,2016,36(8):237ZHANG L,WANG X,XING J,et al.Simultaneous determination of gallic acid,protocatechuic acid,chlorogenic acid,loganin and ferulic acid of herb liquor of Zuogui pills by HPLC[J].Chin JPharm Anal,2016,36(8):237
[9]郝乘仪,昌盛.高效液相色谱法同时测定牛黄清宫丸中5种成分的含量[J].中国医院药学杂志,2017,37(1):80HAO CY,CHANG S.Simultaneous determination of five compounds in Niuhuang Qinggong pills by HPLC[J].Chin J Hosp Pharm,2017,37(1):80
[10]龙厚宁,印酬,孟小夏,等.HPLC同时测定炎热清软胶囊中栀子苷黄芩苷和汉黄芩苷的含量[J].中国实验方剂学杂志,2016,22(6):34LONG HN,YIN C,MENG XX,et al.Simultaneous detemination of geniposide,baicalin and wogonoside inYanreqing soft capsules by HPLC[J].Chin J Exp Tradit Med Form,2016,22(6):34
[11]郭东晓,林林,汪冰,等.HPLC波长切换法同时测定抗感颗粒中7个成分的含量[J].药物分析杂志,2015,35(10):1796GUO DX,LIN L,WANG B,et al.Simultaneous determination of the content of seven components in Kanggan granules by HPLCwavelength switching technology[J].Chin J Pharm Anal,2015,35(10):1796
[12]周军,张蕾,张茉,等.HPLC法同时测定香连化滞丸中7种成分的含量[J].中国药房,2016,27(6):840ZHOU J,ZHANG L,ZHANG M,et al.Contents determination of 7ingredient in Xianglian Huazhi pills by HPLC[J].J China Pharm,2016,27(6):840
[2]范全民.HPLC测定小儿退热口服液中绿原酸与黄芩苷含量[J].现代中药研究与实践,2011,25(2):72FAN QM.Determination of chlorogenic acid and baicalin in Xiaoer Tuire Koufuye by HPLC[J].Res Practic Chin Med,2011,25(2):72
[3]黄海燕,钟建理,钟名诚.HPLC法测定小儿退热口服液中丹皮酚的含量[J].中国药事,2008,22(5):415HUANG HY,ZHONG JL,ZHONG MC.Determination of paeonol in Xiaoer Tuire oral solution by HPLC[J].Chin Pharm Aff,2008,22(5):415
[4]吴丽红,储忠英,刘惠军.HPLC同时测定小儿退热口服液中黄芩苷和丹皮酚的含量[J].中国药师,2013,16(12):1853WU LH,CHU ZY,LIU HJ.Determination of baicalin and paeonol in Xiaoer Tuire oral liquids by HPLC[J].China Pharm,2013,16(12):1853
[5]聂聪珍.高效液相色谱法测定小儿退热合剂中栀子苷的含量[J].中国医药指南,2013,11(14):486NIE CZ.Determination of geniposide in Xiaoer Tuire mixture by HPLC[J].Guide China Med,2013,11(14):486
[6]雷志英,龚建平,彭静.高效液相色谱法同时测定小儿退热口服液中黄芩苷和连翘苷的含量[J].中南药学,2010,8(5):359LEI ZY,GONG JP,PENG J.Determination of baicalin and phillyrin in Xiaoer tuire oral liquid by HPLC[J].Cent South Pharm,2010,8(5):359
[7]张小妹.10批次小儿退烧口服液不符规定被召回[J].广西质量监督导报,2016(1):21ZHANG XM.The tenth batch of Xiaoer Tuire Oral solution is recalled[J].Guangxi Qual Supervis Guide Period,2016(1):21
[8]张琳,汪轩,邢婧,等.HPLC-DAD同时测定左归丸药液中没食子酸、原儿茶酸、绿原酸、马钱苷、阿魏酸含量[J].药物分析杂志,2016,36(8):237ZHANG L,WANG X,XING J,et al.Simultaneous determination of gallic acid,protocatechuic acid,chlorogenic acid,loganin and ferulic acid of herb liquor of Zuogui pills by HPLC[J].Chin JPharm Anal,2016,36(8):237
[9]郝乘仪,昌盛.高效液相色谱法同时测定牛黄清宫丸中5种成分的含量[J].中国医院药学杂志,2017,37(1):80HAO CY,CHANG S.Simultaneous determination of five compounds in Niuhuang Qinggong pills by HPLC[J].Chin J Hosp Pharm,2017,37(1):80
[10]龙厚宁,印酬,孟小夏,等.HPLC同时测定炎热清软胶囊中栀子苷黄芩苷和汉黄芩苷的含量[J].中国实验方剂学杂志,2016,22(6):34LONG HN,YIN C,MENG XX,et al.Simultaneous detemination of geniposide,baicalin and wogonoside inYanreqing soft capsules by HPLC[J].Chin J Exp Tradit Med Form,2016,22(6):34
[11]郭东晓,林林,汪冰,等.HPLC波长切换法同时测定抗感颗粒中7个成分的含量[J].药物分析杂志,2015,35(10):1796GUO DX,LIN L,WANG B,et al.Simultaneous determination of the content of seven components in Kanggan granules by HPLCwavelength switching technology[J].Chin J Pharm Anal,2015,35(10):1796
[12]周军,张蕾,张茉,等.HPLC法同时测定香连化滞丸中7种成分的含量[J].中国药房,2016,27(6):840ZHOU J,ZHANG L,ZHANG M,et al.Contents determination of 7ingredient in Xianglian Huazhi pills by HPLC[J].J China Pharm,2016,27(6):840