CN101699281B - 一种对乙酰半胱氨酸及其有关物质的检测方法 - Google Patents
一种对乙酰半胱氨酸及其有关物质的检测方法 Download PDFInfo
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Abstract
本发明涉及一种对乙酰半胱氨酸及其有关物质的检测方法。该发明采用高效液相色谱法,色谱条件为:苯乙烯-二乙烯基苯共聚物型高聚物色谱柱:MKF-RP-MH,4~10μm,(100~300)×(8.0~4.0)mm(I.D.);流动相组成体积比为0.01~0.05mol/L的磷酸盐缓冲液(pH=2~5)和乙腈的体积比为80~95∶20~5;流速:0.8~1.2mL/min;紫外检测器,检测波长:210nm;进样量:10~20μL。本发明不用离子对试剂,且克服了ODS柱检测法测乙酰半胱氨酸不耐酸、不耐低有机相等缺点。
Description
(一)技术领域
本发明涉及一种高效液相色谱(HPLC)检测方法,具体涉及一种以高聚物(即苯乙烯-二乙烯基苯共聚物,PS-DVB)色谱介质为分离载体装填的色谱柱检测乙酰半胱氨酸及其有关物质的分析检测方法。
(二)背景技术
乙酰半胱氨酸为合成谷胱甘肽的必需氨基酸,是一种含有巯基的抗氧化剂,用于治疗急性、慢性支气管炎以及其他原因引起的粘痰合并发生的肺部疾病。乙酰半胱氨酸还可用于HIV病毒感染者的治疗,改善由于病毒引起的半胱氨酸缺乏患者的生理和免疫功能。
乙酰半胱氨酸在生产过程中容易引入L-胱氨酸、L-半胱氨酸、N,N’-二乙酰胱氨酸和N,S-二乙酰胱氨酸等有关物质。目前各国药典对乙酰半胱氨酸的有关物质均有严格的规定,其中《中国药典》2005版采用碘量法对乙酰半胱氨酸进行含量测定,但未对有关物质进行规定;《美国药典》28版使用HPLC及ODS柱,以苯丙氨酸为内标物,对乙酰半胱氨酸的含量进行测定,也未对有关物质进行规定;《英国药典》2003版使用ODS柱,利用离子对色谱法对乙酰半胱氨酸及其有关物质进行分离,分离效果较好,但流动相使用的离子对试剂(庚烷磺酸钠)较为昂贵,检测成本高,并且流动相pH值较低,也会影响色谱柱使用寿命;另外《中国国家药品标准》(2007年1月1号实施),标准号为:WS1-(X-261)-2003Z-2006)的方法与《英国药典》2003版所述方法基本一致,也需用庚烷磺酸钠;《欧洲药典》52版使用ODS柱,利用离子抑制色谱法对乙酰半胱氨酸及其有关物质进行分析,该方法所用流动相体系较为简单,但该分析方法流动相中有机相比例偏低(仅为3%),低于普通ODS柱承受下限(最低有机相比例为5%),并且流动相pH值也较低,长期使用对色谱柱的寿命有影响。因此开发一种更为适宜的检测方法对于乙酰半胱氨酸及其有关物质的检测具有实际意义。
(三)发明内容
本发明的目的是开发研究一种能对乙酰半胱氨酸及其有关物质进行快速、准确检测的分析检测方法。
本发明的技术方案如下,一种乙酰半胱氨酸及其有关物质高效液相色谱的快速分析检测方法,其特点在于采用一种多孔型聚苯乙烯-二乙烯基苯共聚物为固定相的高聚物色谱柱,高效液相色谱操作条件为:
a.高聚物色谱柱:MKF-RP-MH(南京麦科菲高效分离载体有限公司生产),4~10μm,(100~300)×(8.0~4.6)mm(I.D.);
b.流动相:0.01~0.05mol/L的磷酸盐缓冲液(pH=2~5)和乙腈的体积比为80~95∶20~5;
c.流速:0.8~1.2mL/min,进样量:10~20μL,柱温:室温;
d.采用UV检测器,检测波长为:210nm。
与现有技术相比,本发明的优点和效果如下:
1、选用高聚物色谱柱(MKF-RP-MH)及常规的磷酸盐缓冲液(pH=3.0),乙腈比例为20~5%的范围内,乙酰半胱氨酸以及其有关物质达到了有效的分离,该流动相的pH值以及有机相比例均在所用的MKF-RP-MH柱的适用范围内。
2、该方法与《欧洲药典》52版所述方法的分离效果相当,但本方法所用色谱柱具有更好的酸碱耐受性,更适合在此流动相中长期使用,因而具有更好的实用价值。
3、与《英国药典》28版以及《中国国家药品标准》中所述方法相比,所用流动相条件得到了简化,节省了分析成本,提高了对乙酰半胱氨酸及有关物质检测的灵敏度。
(四)具体实施方案
实验器材及试剂:
(1)实验仪器:
Summit高效液相色谱仪(戴安公司),由P680HPLC泵、UVD-170U可变波长紫外检测器、8125型进样装置组成;工作站(美国戴安Chromeleon系统)。
(2)实验试剂:
乙酰半胱氨酸对照品(上海第一生化药业有限公司),L-胱氨酸(上海惠兴生化试剂有限公司),L-半胱氨酸(上海惠兴生化试剂有限公司),N,N’-二乙酰胱氨酸和N,S-二乙酰胱氨酸(自制)。磷酸二氢钠、磷酸(均为国产分析纯)。
(3)色谱条件:
色谱柱:填料为高度交联的苯乙烯-二乙烯基苯共聚物(PS-DVB)微球,粒径4~10μm,(南京麦科菲高效分离载体有限公司,型号:MKF-RP-MH,(100~300)×(8.0~4.6)mm(I.D.))。流动相:0.01~0.05mol/L的磷酸盐缓冲液-乙腈,流速:0.8~1.2mL/min,进样量:10~20μL,柱温:25℃。
(4)样品配制:
乙酰半胱氨酸供试品溶液的配制:分别精确称量乙酰半胱氨酸、L-胱氨酸、L-半胱氨酸、N,N’-二乙酰胱氨酸和N,S-二乙酰胱氨酸各5mg置于100mL容量瓶中以流动相定容至刻度。
各组分对照品溶液的配制精确称量乙酰半胱氨酸5mg置于100mL容量瓶中以流动相定容至刻度,有关物质对照品溶液同上。
实施例1
色谱条件:检测机器:戴安Summit型高效液相色谱系统;色谱柱:MKF-RP-MH,(250mm×4.6mm,5μm);流动相:0.05mol·L-1的磷酸盐缓冲液(pH=3.0)-乙腈(80∶20);流速:1mL/min;检测波长:254nm;进样量:20μL;进样物质:混合样品。结果:乙酰半胱氨酸及其有关物质均达到了基线分离。
实施例2
色谱条件:检测仪器、色谱柱、检测波长、进样量、进样物质同实施例1,流动相:0.01mol/L的磷酸盐缓冲液(pH=4.0)-乙腈(80∶20);流速:0.8mL/min。结果:乙酰半胱氨酸及其有关物质均达到了基线分离。
实施例3
色谱条件:检测仪器、色谱柱、检测波长、进样量、进样物质同实施例1,流动相:0.03mol/L的磷酸盐缓冲液(pH=4.0)-乙腈(85∶15);流速:0.9mL/min。结果:乙酰半胱氨酸及其有关物质均达到了基线分离。
实施例4
色谱条件:检测仪器、检测波长、流速、进样物质同实施例1,色谱柱:MKF-RP-MH(200mm×7.8mm,5μm),进样量:10μL;流动相:0.01mol/L的磷酸盐缓冲液(pH=3.0)-乙腈(90∶10)。结果:乙酰半胱氨酸及其有关物质均达到了基线分离。
实施例5
色谱条件:检测仪器、检测波长、进样量、进样物质同实施例1,色谱柱:MKF-RP-MH(200mm×7.8mm,10μm),流动相:0.04mol/L的磷酸盐缓冲液(pH=2.0)-乙腈(95∶5),流速:0.9ml/min。结果:乙酰半胱氨酸及其有关物质均达到了基线分离。
实施例6
色谱条件:检测仪器、检测波长、流速、进样量、进样物质同实施例1,色谱柱:MKF-RP-MH(250mm×4.6mm,6μm),流动相:0.05mol/L的磷酸盐缓冲液(pH=4.0)-乙腈(85∶15)。结果:乙酰半胱氨酸及其有关物质均达到了基线分离。
实施例7
色谱条件:检测仪器、检测波长、流速、进样量、进样物质同实施例1,色谱柱:MKF-RP-MH(300mm×7.8mm,8μm),流动相:0.03mol/L的磷酸盐缓冲液(pH=5.0)-乙腈(90∶10)。结果:乙酰半胱氨酸及其有关物质均达到了基线分离。
实施例8
色谱条件:检测仪器、检测波长、进样量、进样物质同实施例1,色谱柱:MKF-RP-MH(250mm×4.6mm,4μm),流动相:0.01mol/L的磷酸盐缓冲液(pH=3.5)-乙腈(85∶15),流速:1.1ml/min。结果:乙酰半胱氨酸及其有关物质均达到了基线分离。
实施例9
色谱条件:检测仪器、检测波长、进样量、进样物质同实施例1,色谱柱:MKF-RP-MH(250mm×4.6mm,8μm),流动相:0.02mol/L的磷酸盐缓冲液(pH=5)-乙腈(80∶20),流速:1.2ml/min。结果:乙酰半胱氨酸及其有关物质均达到了基线分离。
实施例10
色谱条件:检测仪器、检测波长、流速、进样量、进样物质同实施例1,色谱柱:MKF-RP-MH(250mm×4.6mm,5μm),流动相:0.01mol/L的磷酸盐缓冲液(pH=5.0)-乙腈(80∶20)。结果:乙酰半胱氨酸及其有关物质均达到了基线分离。
Claims (3)
1.一种高效液相色谱法测定乙酰半胱氨酸及其有关物质的方法,其特征在于选用聚苯乙烯型-高聚物色谱柱,以磷酸盐缓冲液与乙腈为流动相,分离乙酰半胱氨酸及其有关物质;
其所述的聚苯乙烯型-高聚物色谱柱为MKF-PR型色谱柱,其色谱柱规格为4~10μm,(100~300)×(8.0~4.6)mm(I.D.),或为8~10μm,250×4.6mm(I.D.);
流动相中磷酸盐缓冲液的含量为0.01~0.05mol.L-1,pH为2~5,及磷酸盐缓冲液与乙腈的体积比为80~95:20~5;
其所述的有关物质为:L-胱氨酸、L-半胱氨酸、N,N’-二乙酰胱氨酸和N,S-二乙酰胱氨酸。
2.根据权利要求1所述的一种高效液相色谱法测定乙酰半胱氨酸及其有关物质的方法,其特征在于,选用流速为:0.8~1.2mL/min。
3.根据权利要求1所述的一种高效液相色谱法测定乙酰半胱氨酸及其有关物质的方法,其特征在于,采用UV检测器,检测波长为210nm。
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CN103323553B (zh) * | 2013-07-01 | 2015-10-21 | 华仁药业股份有限公司 | 一种器官保存液中乙酰半胱氨酸有关物质的定量检测方法 |
CN104142370B (zh) * | 2014-01-03 | 2016-01-06 | 南京工业大学 | 一种1-苯基-2-硝基丙烯及其相关物质的分析检测方法 |
CN105181859A (zh) * | 2015-10-12 | 2015-12-23 | 南京天翔医药科技有限公司 | 对乙酰氨基酚注射液中盐酸半胱氨酸及降解产物胱氨酸的测定方法 |
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