在线2D-LC-QTOF MS识别氨基葡萄糖液相色谱中可疑色谱峰
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- 英文论文题名：Online 2D-LC-QTOF MS to profile suspicious peaks in HPLC for determining glucosamine
- 论文作者：徐明明 ; 郑璐侠 ; 汪泓 ; 邵泓 ; 刘国强 ; 陈钢
- 英文论文作者：XU Ming-ming ; ZHENG Lu-xia ; WANG Hong ; SHAO Hong ; Liu Guo-qiang ; CHEN Gang ; Shanghai Institute for Food and Drug Control ; Agilent Technologies(China)Co. ; Ltd.
- 年：2016
- 作者机构：上海市食品药品检验所;安捷伦科技(中国)有限公司;
- 论文关键词：2D-LC-QTOF MS ; 液相色谱法 ; 氨基葡萄糖 ; 氯离子 ; 硫酸根离子
- 英文论文关键词：2D-LC-QTOF MS ; HPLC ; glucosamine ; Cl~- ; SO_4~(2-)
- 会议召开时间：2016-09-27
- 会议录名称：中国药学会第十三届青年药学科研成果交流会论文集
- 语种：中文
- 分类号：R927;O657.63
- 学会代码：YYWS
- 会议名称：中国药学会第十三届青年药学科研成果交流会
- 会议地点：中国江西南昌
- 主办单位：中国药学会
- 学会名称：中国药学会
- 页数：6
- 文件大小：357k
- 原文格式：O
- 会议级别：全国
摘要
建立在线二维液相色谱-四极杆飞行时间质谱法(2D-LC-QTOF MS)对氨基葡萄糖液相色谱中3个可疑色谱峰进行结构分析。第一维HPLC以Inertsil C8-3为色谱柱,以磷酸盐缓冲液(pH 2.5)-乙腈(80:20)为流动相进行洗脱,第二维HPLC以Poroshell 120 EC-C18为色谱柱,以0.1%(v/v)甲酸水溶液和0.1%(v/v)甲酸乙腈溶液为流动相进行梯度洗脱。当第一维HPLC目标组分出峰时,通过阀切换将目标组分准确切割并捕获在40μL定量环中,之后第二维HPLC泵将捕获的组分洗脱进行质谱检测。采用正负离子模式采集数据,对第一维谱图中3个色谱峰进行了结构分析,鉴定其分别为氨基葡萄糖、硫酸根离子和氯离子。结果确定第一维HPLC测定的主峰为氯离子,而非活性组分氨基葡萄糖,该方法专属性差,采用该液相含量测定方法的进口药品注册标准和国家药品标准不能控制该类药品的有效性,标准亟需改进和提高。
A 2D-LC-QT0 F MS method to profile three peaks in HPLC for determining glucosamine was developed.A Inertsil C8 column(250 mm × 4.6 mm,5 μm) was used in the first dimensional chromatography,using pH 2.5 phosphate buffer and acetonitrile(80:20) as the mobile phase.The column temperature was maintained at 30 ℃ with an ultraviolet detection of 195 nm for analysis.An Poroshell EC-C18 column(100mm × 3.0mm,2.7 μm) was used in the second dimensional chromatography,with gradient elution using water containing 0.1%(v/v) formic acid and acetonitrile containing 0.1%(v/v) formic acid as the mobile phase.The column temperature was maintained at 30 ℃.The target peak from the first dimensional LC was trapped in 40 μL loop via switching valve,and then was separated using a MS compatible mobile phase from Pump 2.The data was collected in positive and negative ion mode.The ion source was Dual AJS ESI,and the temperature of dry gas was set at 300 ℃ and the electrospray ionization(ESI) needle voltage was set at 3000 V.The nebulizer gas was set at 350 ℃.The molecular formulas were determined by their exact masses and isotope distributions.Three peaks in HPLC were glucosamine,SO_4~(2-) and Cl~-.The main peak is Cl~- in HPLC for determining glucosamine,but not the active ingredient of glucosamine.The standards of registration of imported drug and national drug using the HPLC method above for the determination of glucosamine can't control the effectiveness of the products,because of HPLC method are lack of specificity.And the standards need to be improved.
A 2D-LC-QT0 F MS method to profile three peaks in HPLC for determining glucosamine was developed.A Inertsil C8 column(250 mm × 4.6 mm,5 μm) was used in the first dimensional chromatography,using pH 2.5 phosphate buffer and acetonitrile(80:20) as the mobile phase.The column temperature was maintained at 30 ℃ with an ultraviolet detection of 195 nm for analysis.An Poroshell EC-C18 column(100mm × 3.0mm,2.7 μm) was used in the second dimensional chromatography,with gradient elution using water containing 0.1%(v/v) formic acid and acetonitrile containing 0.1%(v/v) formic acid as the mobile phase.The column temperature was maintained at 30 ℃.The target peak from the first dimensional LC was trapped in 40 μL loop via switching valve,and then was separated using a MS compatible mobile phase from Pump 2.The data was collected in positive and negative ion mode.The ion source was Dual AJS ESI,and the temperature of dry gas was set at 300 ℃ and the electrospray ionization(ESI) needle voltage was set at 3000 V.The nebulizer gas was set at 350 ℃.The molecular formulas were determined by their exact masses and isotope distributions.Three peaks in HPLC were glucosamine,SO_4~(2-) and Cl~-.The main peak is Cl~- in HPLC for determining glucosamine,but not the active ingredient of glucosamine.The standards of registration of imported drug and national drug using the HPLC method above for the determination of glucosamine can't control the effectiveness of the products,because of HPLC method are lack of specificity.And the standards need to be improved.
引文
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[2]Liu L P,Zhang F F,Zhang Y,et al.ACTA Nutrimenta SINICA(刘利萍,章非凡,张阳,等.营养学报),2013,35(4):387
[3]Di PR Lao Y Z,Zhao L R et a1.Chinese Pharmaceufical Affairs(狄平平,劳苑子,赵立平,等.中国药事),2010,24(3):283
[4]Huang X,Chen Q S,Xu J Z,et a1.Journal of Fujian Normal University(黄鑫,陈清松,许建中,等.福建师范大学学报)I 2009,25(3):80
[5]Zai Z L,Yang R C,Wang A Y.Chinese Journal ofHealth Laboratory Technology(翟志雷,杨瑞春,王爱月.中国卫生检验杂志),2010,20(6):1380
[6]Cu L M,Xu J G.Huo L R.Journal ofPediatric Pharmacy(初立梅,徐家根,霍立茹.儿科药学杂志),2012,18(3):40
[7]Liao X,Wang S J,Tong Y,et al.Journal of Shenyang Pharmaceutical University(廖栩,王淑君,佟岩,等.沈阳药科大学学报),2011,28(5):380
[8]Wan H F,Wan X,Wang H J.Journal of Nanchang University(万慧芳,万欢,汪华杰.南昌大学学报),2010,50(5):96
[9]Hong Z,Huang H N,Xu C,et al.Chinese Journal of Health Laboratory Technology(洪专,黄宏南,许晨,等.中国卫生检验杂志),2007,17(6):1025
[10]Jiang H,Dan X M,Hu Y H,et al.Drug Standard of China(姜红,但晓梦,胡远华,等.中国药品标准),2013,14(4):259
[11]Shen G,Xu J Z,Tang X,et al.Chinese Journal of Health Laboratory Technology(沈国,许建中,唐旭,等.中国卫生检验杂志),2010,20(3):495
[12]Zhang S W,Zheng B,Zhou X L,et al.Chinese Journal of Chromatography(张思维,郑波,皱晓丽,等.色谱),2009,27(1):117
[13]Gan BB,Liu ZH,Li SH.Chinese Journal of Food hygiene(甘宾宾,刘展华,黎少豪.中国食品卫生杂志),2011,23(6):531
[14]Zhang J L,He Z Y,Yin Y J.Heilongjiang Medicine Journal(张佳蕊,何志一,尹燕杰.黑龙江医药),2013,26(3):353
[15]Yang L,Li T L,Huang T,et al.West China Journal of Pharmaceutical Sciences(杨岚,李铜铃,黄婷,等.华西药学杂志),2005,20(3):259
[16]Luo L,Dan H X.China pharmacist(罗立,但汉雄.中国药师),2016,19(2):387
[17]Zeng M F,Li J,Wang YY,etal.Chinese Journal of Modern Applied Pharmacy(曾茂法,李俊,王英瑛,等.中国现代应用药学杂志),2008,25(3):251
[18]Liu S T,Li S,Ym H P,et al.Chin J Pharm Anal(刘升涛,李师,尹鸿萍,等.药物分析杂志),2015,35(5):900
[19]Yang HL,Lei YS.Tianjin Pharmacy(杨华良,雷勇胜.天津药学),2011,23(6):17
[20]USP,2016,39:6677
[21]Dan X M.The research in quality control of glucosamine drugs.Wuhan,2012:1
[22]Chen W Z,Zhang Y P.Fang H,et al.Chemical Analysis and Meterage(陈伟珠,张怡评,方华,等.化学分析计量),2015,24(2):l
[23]Zhang H J,Zhang Z,Zhang R.Chinese Journal of Health Laboratory Technology(张华瑁,张拮,张蓉.中国卫生检验杂志),2013,23(5):1148
[24]Qiu Y,Qin F,Wen H L,et al.Chinese Journal of Chromatography(裘亚,秦峰,闻宏亮,等.色谱),2015,33(12):1314