CN112798710A - 一种检测人血浆左乙拉西坦浓度的hplc-uv方法 - Google Patents
一种检测人血浆左乙拉西坦浓度的hplc-uv方法 Download PDFInfo
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Abstract
本发明公开了一种检测人血浆左乙拉西坦浓度的HPLC‑UV方法,本发明通过采用甲醇直接沉淀蛋白法结合HPLC‑UV检测人血浆左乙拉西坦浓度,只需要极少量血浆即可检测左乙拉西坦浓度,线性范围2‑100μg/mL(R2>0.99),批内与批间精密度均≤3.58%,准确度范围是96.09%‑97.86%,本发明检测限低、选择性佳且具有极好的特异性和灵敏度,整个检测时间短,残留、干扰及提取回收率都满足要求,同时具有检测结果稳定的优点。
Description
技术领域
本发明涉及医疗技术领域,具体为一种检测人血浆左乙拉西坦浓度的HPLC-UV方法。
背景技术
左乙拉西坦是一种新型的抗癫痫药,可用于部分癫痫发作的单一治疗,也可作为部分、肌阵挛和原发性全身强直阵挛发作的辅助治疗,2007年引入中国。其结构和抗癫痫的机制与其他药物不同,主要是选择性地抑制癫痫样突发放电的超同步性和癫痫发作的传播而发挥作用。左乙拉西坦的药代动力学在儿童和成人之间有所不同,吸收、分布、代谢和排泄的药代动力学过程随着生长发育而发生变化。虽然左乙拉西坦容易服用且耐受,但在很多临床治疗中需要进行药物监测(怀疑不遵从、怀孕、儿童剂量、肾衰竭和高剂量无效)。目前左乙拉西坦的测定方法推荐采用HPLC法或者LC-MS/MS法,LC-MS/MS法样本前处理复杂且耗时,仪器昂贵,难以普及应用于日常临床。因此有必要开发一种采用HPLC法且简单便捷的检测方法。
发明内容
本发明的目的在于,提供一种检测人血浆左乙拉西坦浓度的HPLC-UV方法。本发明具有检测快捷、灵敏性和特异性高的优点。
本发明的技术方案:一种检测人血浆左乙拉西坦浓度的HPLC-UV方法,按以下步骤进行:
S1:色谱条件:色谱柱:Diamonsil C18 column,150mm×4.6mm ID,5μm;流动相:乙腈与10mM磷酸二氢钾的比为10:90;流速:1mL/min;柱温:35℃;进样体积:15μL;检测波长:210nm;
S2:溶液配制:称取左乙拉西坦标准品,用甲醇溶解,得到浓度1.0mg/mL的左乙拉西坦储备液,置4℃下冷藏备用;
S3:取左乙拉西坦储备液,用甲醇按比例稀释成系列标准溶液,再加入空白血浆制成左乙拉西坦标准曲线血浆样品;所述左乙拉西坦标准曲线的血浆样品浓度分别为:2μg/mL、5μg/mL、10μg/mL、20μg/mL、50μg/mL、70μg/mL和100μg/mL;再分别取50μL血浆样品,加入150μL甲醇,涡旋混匀1min,于15000r高速离心10min,取上清液15μL进行色谱进样;
S4:对步骤S3进行色谱进样的7个浓度点采用1/x加权进行线性回归,即左乙拉西坦的峰面积对样品浓度采取最小二乘法,得到左乙拉西坦标准曲线回归方程:
y=2.16×10-4x+0.816,(r2=0.998);
式中:y为血浆左乙拉西坦浓度,x为左乙拉西坦峰面积;
S5:取左乙拉西坦储备液,用甲醇按比例稀释成系列标准溶液,再加入空白血浆制成高中低血浆质控样本;所述血浆质控样本浓度分别为4μg/mL、35μg/mL和80μg/mL,再分别取50μL血浆质控样本,加入150μL甲醇,涡旋混匀1min,于15000r高速离心10min,取上清液15μL进行色谱进样;连续检测3天,计算日内和日间精密度;
S6:取左乙拉西坦储备液,用甲醇按比例稀释成浓度分别为4μg/mL、35μg/mL和80μg/mL的标准溶液各5份,再分别取50μL标准溶液,加入150μL甲醇,涡旋混匀1min,于15000r高速离心10min,取上清液15μL进行色谱进样;检测后比较S4步骤中的峰面积与本步骤中的峰面积之比,作提取回收率。
上述的检测人血浆左乙拉西坦浓度的HPLC-UV方法,步骤S4中,根据RSN=10及临床诊断要求确定血浆左乙拉西坦浓度的最低定量限为2μg/mL。
与现有技术相比,本发明通过采用甲醇直接沉淀蛋白法结合HPLC-UV检测人血浆左乙拉西坦浓度,具有检测快捷、灵敏性和特异性高的优点。本发明可以检测患者左乙拉西坦血药浓度,避免临床用药疗效不佳或发生不良反应,为临床提供优化的给药方案,为患者个体化用药提供可靠的实验依据。实验结果表明,本发明只需要极少量血浆即可检测左乙拉西坦浓度,线性范围2-100μg/mL(R2>0.99),批内与批间精密度均≤3.58%,准确度范围是96.09%-97.86%,本发明检测限低、选择性佳且具有极好的特异性和灵敏度,整个检测时间短,残留、干扰及提取回收率都满足要求,同时具有检测结果稳定的优点。
附图说明
图1为空白血浆色谱图;
图2为空白血浆加左乙拉西坦标准品色谱图;
图3为患者血浆色谱图;
图4是图1、图2和图3的色谱图进行叠加的示意图。
具体实施方式
下面结合附图和实施例对本发明作进一步的说明,但并不作为对本发明限制的依据。
实施例:一种检测人血浆左乙拉西坦浓度的HPLC-UV方法,本实施采用的仪器包括:
HPLC-UV系统:e2695高效液相色谱仪(Waters,美国)和2489紫外检测器(Waters,美国);
EmpowerTM(Waters,美国);
Forma-86C超低温冰箱(Thermo,美国);
SL102N电子天平(MINQIAO,中国);
XP26微量分析天平(梅特勒-托利多,瑞士);
Allegra 6R、64R超高速低温离心机(Beckman,美国);
MS3 basic漩涡仪(IKA,德国);
溶剂过滤器(津腾,中国)。
该技术检测左乙拉西坦浓度的标准品和试剂包括:
左乙拉西坦对照品(Toronto Research Chemicals Inc,批号:3-JSH-3-1,CAS:102767-28-2,含量98%);
乙腈(HPLC级,Merck公司);
甲醇(HPLC级,Merck公司);
磷酸二氢钾(HPLC级,广东省化学试剂工程技术研究开发中心);
Milli-Q超纯水(自制)。
按以下步骤进行:
S1:色谱条件:色谱柱:Diamonsil C18 column,150mm×4.6mm ID,5μm;流动相:乙腈与10mM磷酸二氢钾的比为10:90(质量比);流速:1mL/min;柱温:35℃;进样体积:15μL;检测波长:210nm;
S2:溶液配制:精密称取2.35mg左乙拉西坦标准品,用甲醇溶解,得到浓度1.0mg/mL的左乙拉西坦储备液,置4℃冰箱内冷藏备用;
S3:取左乙拉西坦储备液,用甲醇按比例稀释成系列标准溶液,再加入空白血浆制成左乙拉西坦标准曲线血浆样品,左乙拉西坦标准曲线的血浆样品浓度分别为:2μg/mL、5μg/mL、10μg/mL、20μg/mL、50μg/mL、70μg/mL和100μg/mL;再分别取50μL血浆样品,加入150μL甲醇,涡旋混匀1min,于15000r高速离心10min,取上清液15μL进行色谱进样;如图1和如2所示,左乙拉西坦的保留时间为4.7min,随机考察6份不同的空白血浆以及加左乙拉西坦标准品的血浆,结果分别如图1和图2所示,从图1和图2中可以看出空白血浆色谱分离良好,内源性物质均不干扰左乙拉西坦的出峰;
S4:对步骤S3进行色谱进样的7个浓度点采用1/x加权进行线性回归,即左乙拉西坦的峰面积对样品浓度采取最小二乘法,得到左乙拉西坦标准曲线回归方程:
y=2.16×10-4x+0.816,(r2=0.998);
式中:y为血浆左乙拉西坦浓度,x为左乙拉西坦峰面积;
根据RSN=10及临床诊断要求确定血浆左乙拉西坦浓度的最低定量限为2μg/mL;
S5:取左乙拉西坦储备液,用甲醇按比例稀释成系列标准溶液,再加入空白血浆制成高中低血浆质控样本,血浆质控样本浓度分别为4μg/mL、35μg/mL和80μg/mL,再分别取50μL血浆质控样本,加入150μL甲醇,涡旋混匀1min,于15000r高速离心10min,取上清液15μL进行色谱进样;连续检测3天,计算日内和日间精密度(按上面公式代入峰面积得浓度,按浓度结果分析得到精密度);
S6:取左乙拉西坦储备液,用甲醇按比例稀释成浓度分别为4μg/mL、35μg/mL和80μg/mL的标准溶液各5份,再分别取50μL标准溶液,加入150μL甲醇,涡旋混匀1min,于15000r高速离心10min,取上清液15μL进行色谱进样;检测后比较S4步骤中的峰面积与本步骤中的峰面积之比,作提取回收率。
具体的,本发明测定的精密度和回收率表1所示:
表1
表中:Conc.μg/mL:浓度(μg/mL);Inter-day precision:日内精密度;Intra-dayprecision:日间精密度;Extraction recovery:回收率;Mean±SD:均值±标准差;RSD:变异系统。
申请人还将血浆样品室温放置6小时、上清液样品在自动进样器放置24小时、血浆样品三次冻融循环、血浆样品在-20℃存放30天和-80℃存放95天,再分别取50μL,加入150μL甲醇,涡旋混匀1min,于15000r高速离心10min,取上清液15μL进行色谱进样;新鲜配制一条标准曲线来评价准确度,同浓度检测的均值与理论值之间的浓度偏差均≤15%。
进一步地,申请人利用本发明对患者血浆中左乙拉西坦浓度进行实际检测,结果如图3所示,将图1-图3进行叠加得到如图4所示的叠加效果图,从图3和图4可以看到,本发明可以准确的检测出患者的血浆中左乙拉西坦浓度,具有检测快捷、灵敏性和特异性高的优点。
综上所述,本发明只需要极少量血浆即可检测左乙拉西坦浓度,经试验证明,本发明的线性范围2-100μg/mL(R2>0.99),批内与批间精密度均≤3.58%,准确度范围是96.09%-97.86%,本发明检测限低、选择性佳且具有极好的特异性和灵敏度,整个检测时间短,残留、干扰及提取回收率都满足要求,同时具有检测结果稳定的优点。
Claims (2)
1.一种检测人血浆左乙拉西坦浓度的HPLC-UV方法,其特征在于:按以下步骤进行:
S1:色谱条件:色谱柱:DiamonsilC18 column,150mm×4.6mm ID,5μm;流动相:乙腈与10mM磷酸二氢钾的比为10:90;流速:1mL/min;柱温:35℃;进样体积:15μL;检测波长:210nm;
S2:溶液配制:称取左乙拉西坦标准品,用甲醇溶解,得到浓度1.0mg/mL的左乙拉西坦储备液,置4℃下冷藏备用;
S3:取左乙拉西坦储备液,用甲醇按比例稀释成系列标准溶液,再加入空白血浆制成左乙拉西坦标准曲线血浆样品;所述左乙拉西坦标准曲线的血浆样品浓度分别为:2μg/mL、5μg/mL、10μg/mL、20μg/mL、50μg/mL、70μg/mL和100μg/mL;再分别取50μL血浆样品,加入150μL甲醇,涡旋混匀1min,于15000r高速离心10min,取上清液15μL进行色谱进样;
S4:对步骤S3进行色谱进样的7个浓度点采用1/x加权进行线性回归,即左乙拉西坦的峰面积对样品浓度采取最小二乘法,得到左乙拉西坦标准曲线回归方程:
y=2.16×10-4x+0.816,(r2=0.998);
式中:y为血浆左乙拉西坦浓度,x为左乙拉西坦峰面积;
S5:取左乙拉西坦储备液,用甲醇按比例稀释成系列标准溶液,再加入空白血浆制成高中低血浆质控样本;所述血浆质控样本浓度分别为4μg/mL、35μg/mL和80μg/mL,再分别取50μL血浆质控样本,加入150μL甲醇,涡旋混匀1min,于15000r高速离心10min,取上清液15μL进行色谱进样;连续检测3天,计算日内和日间精密度;
S6:取左乙拉西坦储备液,用甲醇按比例稀释成浓度分别为4μg/mL、35μg/mL和80μg/mL的标准溶液各5份,再分别取50μL标准溶液,加入150μL甲醇,涡旋混匀1min,于15000r高速离心10min,取上清液15μL进行色谱进样;检测后比较S4步骤中的峰面积与本步骤中的峰面积之比,作提取回收率。
2.根据权利要求1所述的检测人血浆左乙拉西坦浓度的HPLC-UV方法,其特征在于:步骤S4中,根据RSN=10及临床诊断要求确定血浆左乙拉西坦浓度的最低定量限为2μg/mL。
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