CN111458432B - 一种高效液相色谱法检测三氟乙酰乙酸乙酯的方法 - Google Patents
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Abstract
本发明涉及化工分析技术领域,具体涉及一种高效液相色谱法检测三氟乙酰乙酸乙酯的方法,包括(1)标准品溶液的配制:称取适量的三氟乙酰乙酸乙酯标准品溶解于乙腈中,定容,得三氟乙酰乙酸乙酯标准品溶液备用;(2)样品溶液的配制:称取适量的三氟乙酰乙酸乙酯样品溶解于乙腈中,定容,得三氟乙酰乙酸乙酯样品溶液备用;(3)测定:取三氟乙酰乙酸乙酯标准品溶液和样品溶液,注入高效液相色谱仪,进行高效液相色谱分析;其中,高效液相色谱条件包括:采用反向色谱柱,流动相为有机相‑水相,检测波长为227nm,柱温为40℃。该检测方法的线性、范围、回收率及精密度等试验均良好,色谱柱柱稳定性好,且流动相配制简单、检测成本低。
Description
技术领域
本发明涉及化工分析技术领域,具体涉及一种高效液相色谱法检测三氟乙酰乙酸乙酯的 方法。
背景技术
三氟乙酰乙酸乙酯是一种重要的有机化工原料,作为精细中间体,在有机氟化合物合成、 农药、医药、染料以及液晶等行业有着广泛的用途。我国是萤石主要产出国,在原料上有优 势,使得我国成为三氟乙酰乙酸乙酯的主要生产国。
三氟乙酰乙酸乙酯因其极性大,使用液相色谱检测时经常与倒峰、溶剂峰或者杂质峰同 时出峰,且其紫外吸收较弱,当前检测主要以气相检测为主,然而现阶段还没有统一的三氟 乙酰乙酸乙酯检测标准,企业通常使用气相归一法指定内控指标。归一法对所有组分必须在一个分析周期内都流出色谱柱的限制,及会受到出峰效果等原因影响,使归一峰面积变化并 不能完全代表含量的变化,归一变化很小而实际含量变化很大或者归一变化很大而实际含量 变化很小的现象经常出现。
基于此,十分有必要提出一种利用液相色谱法对三氟乙酰乙酸乙酯进行快速高效检测的 方法。
发明内容
针对液相检测三氟乙酰乙酸乙酯时易出现三氟乙酰乙酸乙酯与倒峰、溶剂峰或者杂质峰 同时出峰的技术问题,本发明提供一种高效液相色谱法检测三氟乙酰乙酸乙酯的方法,该检 测方法的线性、范围、回收率及精密度等试验均良好,色谱柱柱稳定性好,且流动相配制简单、检测成本低。
一种高效液相色谱法检测三氟乙酰乙酸乙酯的方法,所述方法包括如下步骤:
(1)标准品溶液的配制:
称取适量的三氟乙酰乙酸乙酯标准品溶解于乙腈中,定容,得三氟乙酰乙酸乙酯标准品 溶液备用;
(2)样品溶液的配制:
称取适量的三氟乙酰乙酸乙酯样品溶解于乙腈中,定容,得三氟乙酰乙酸乙酯样品溶液 备用;
(3)测定:
取三氟乙酰乙酸乙酯标准品溶液和样品溶液,注入高效液相色谱仪,进行高效液相色谱 分析;
其中,高效液相色谱条件包括:
采用反相色谱柱,流动相为有机相-水相,检测波长为227nm,柱温为40℃。
进一步的,所述反相色谱柱为C18柱,优选为博纳艾杰尔Agela色谱柱DurashellC18。
本发明选用的Durashell C18色谱柱通过多官能团键合技术,在硅胶表面覆盖一种强疏水 性保护层,能有效防止碱性溶液对硅胶基质的破坏,因此Durashell C18色谱柱可在高pH下 使用,并且对碱性化合物有极高的载样量,非常适合碱性化合物的制备分离;同时多官能团 键合技术可以减弱固定相和化合物间的疏水相互作用,保持高界面动力学系数,从而获得更高的柱效。开创性使用博纳艾杰尔Agela色谱柱Durashell C18,可以实现三氟乙酰乙酸乙酯 的有效保留,从而避免溶剂峰、倒峰、杂质峰干扰,能够实现快速准确检测。
进一步的,所述流动相中有机相与水相的体积比为50:50。
进一步的,所述流动相中有机相为乙腈,水相为冰乙酸水溶液。选用乙腈溶样,可挥发 性溶液做流动相,可有效避免对色谱柱的损坏,并有效避免流动相或溶剂在短波下的吸收对 样品检测的干扰,更好地实现三氟乙酰乙酸乙酯的质量控制,提高分析的准确性。
进一步的,所述流动相为直接采用双泵分别单独进有机相和水相。流动相中水相和有机 相无需预混,即不需要提前将有机相和水相按比例混合均匀再使用。
进一步的,高效液相色谱条件还包括:流速为1.0mL/min。
进一步的,高效液相色谱条件还包括:进样量为10μL。
进一步的,高效液相色谱条件还包括:洗脱时间为8min。
本发明的有益效果在于,
本发明提供一种高效液相色谱法检测三氟乙酰乙酸乙酯的方法,检测的线性、范围、回 收率及精密度等试验均良好;所选色谱柱柱稳定性好;且流动相配制简单、检测成本低。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案,下面将对实施例或现有技术 描述中所需要使用的附图作简单地介绍,显而易见地,对于本领域普通技术人员而言,在不 付出创造性劳动的前提下,还可以根据这些附图获得其他的附图。
图1是实施例1中样品色谱图;
图2是验证例3中浓度(mg/100mL)-峰面积的线性关系图。
具体实施方式
为了使本技术领域的人员更好地理解本发明中的技术方案,下面将结合本发明实施例中 的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅 是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都应当属于本发明保护的范围。
实施例1
一种高效液相色谱法检测三氟乙酰乙酸乙酯的方法,所述方法包括如下步骤:
(1)标准品溶液的配制:
准确称取三氟乙酰乙酸乙酯0.5g(精确至0.0002g)的标准品,置于100mL容量瓶中,加乙 腈90mL,经超声波振荡溶解,冷却至室温,用乙腈稀释至刻度,摇匀备用,其中标准品中三 氟乙酰乙酸乙酯的含量p1为96.5%;
(2)样品溶液的配制:
准确称取三氟乙酰乙酸乙酯0.05g(精确至0.0002g)的样品,置于100mL容量瓶中,加乙 腈90mL,经超声波振荡溶解,冷却至室温,用乙腈稀释至刻度,摇匀备用;
(3)测定:
测试条件为采用博纳艾杰尔Agela色谱柱Durashell C18,流动相中乙腈与冰乙酸水溶液 的体积比为50:50,检测波长为227nm,柱温为40℃,流速为1.0mL/min,进样量为10μL, 洗脱时间为8min;
待仪器基线稳定后,连续注入数针标样溶液,直至相邻两针三氟乙酰乙酸乙酯响应值相 对变化小于0.5%后,按照标样溶液、试样溶液、试样溶液、标样溶液的顺序进行测定,测试 结果如图1及表1所示。
表1测试数据
采用如下公式(1)计算样品溶液中三氟乙酰乙酸乙酯的含量p2:
式中:
A1——标准品溶液中三氟乙酰乙酸乙酯色谱峰面积的平均值;
A2——样品溶液中三氟乙酰乙酸乙酯色谱峰面积的平均值;
m1——三氟乙酰乙酸乙酯标准品的质量,g;
m2——三氟乙酰乙酸乙酯样品的质量,g。
计算得样品中三氟乙酰乙酸乙酯的含量为96.03%。
验证例1方法的精确度验证
测试条件为采用博纳艾杰尔Agela色谱柱Durashell C18,流动相中乙腈与冰乙酸水溶液 的体积比为50:50,检测波长为227nm,柱温为40℃,流速为1.0mL/min,进样量为10μL, 洗脱时间为8min;
精确度测试结果如下表2所示。
表2精确度测试结果
验证例2方法的准确度验证
采用加标回收实验检测本方法准确度,准确度测试结果如下表3所示。
表3准确度测试结果
验证例3方法的线性关系验证
浓度(mg/100mL)-峰面积的线性关系如图2所示,R2=0.999。
尽管通过参考附图并结合优选实施例的方式对本发明进行了详细描述,但本发明并不限 于此。在不脱离本发明的精神和实质的前提下,本领域普通技术人员可以对本发明的实施例 进行各种等效的修改或替换,而这些修改或替换都应在本发明的涵盖范围内/任何熟悉本技术 领域的技术人员在本发明揭露的技术范围内,可轻易想到变化或替换,都应涵盖在本发明的 保护范围之内。因此,本发明的保护范围应以权利要求所述的保护范围为准。
Claims (2)
1.一种高效液相色谱法检测三氟乙酰乙酸乙酯的方法,其特征在于,所述方法包括如下步骤:
(1)标准品溶液的配制:
称取适量的三氟乙酰乙酸乙酯标准品溶解于乙腈中,定容,得三氟乙酰乙酸乙酯标准品溶液备用;
(2)样品溶液的配制:
称取适量的三氟乙酰乙酸乙酯样品溶解于乙腈中,定容,得三氟乙酰乙酸乙酯样品溶液备用;
(3)测定:
取三氟乙酰乙酸乙酯标准品溶液和样品溶液,注入高效液相色谱仪,进行高效液相色谱分析;
其中,高效液相色谱条件包括:
采用反相色谱柱,所述反相色谱柱为博纳艾杰尔Agela色谱柱DurashellC18,流动相为有机相-水相,所述流动相中有机相为乙腈,水相为冰乙酸水溶液,有机相与水相的体积比为50:50,检测波长为227nm,柱温为40℃,流速为1.0mL/min,进样量为10μL,洗脱时间为8min。
2.如权利要求1所述的高效液相色谱法检测三氟乙酰乙酸乙酯的方法,其特征在于,所述流动相为直接采用双泵分别单独进有机相和水相。
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