CN110208404A - 一种丙硫菌唑中杂质的定性分析方法 - Google Patents
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Abstract
本发明提供一种丙硫菌唑中杂质的定性分析方法，涉及药物检测技术领域，包括如下步骤：S1.取丙硫菌唑中杂质对照品和丙硫菌唑原料药，配制丙硫菌唑中杂质对照品溶液和供试品溶液；S2.色谱检测条件为：以水为流动相A，以乙腈水溶液为流动相B，流动相B中加入乙酸，流速为0.3‑0.5mL/min；梯度洗脱程序为：0‑1min，流动相B的体积百分数为20％；1‑12min，流动相B的体积百分数由20％至30％；12‑18min，流动相B的体积百分数为30％；18‑18.1min，流动相B的体积百分数由30％至20％；18.1‑23min，流动相B的体积百分数为20％；质谱检测条件为：离子流数据采集范围为150‑500Da，离子源温度为110‑130℃，离子传输管温度为300‑500℃，喷雾电压为2‑4KV。本发明操作简单，准确度高。
Description
技术领域
本发明属于药物检测技术领域，本发明涉及一种丙硫菌唑中杂质的定性分析方法。
背景技术
丙硫菌唑是拜耳公司研制的一种新型广谱三唑硫酮类杀菌剂，主要用于防治谷类、麦类豆类作物等众多病害，丙硫菌唑毒性低，无致畸，致突变型，对胚胎无毒性，对人和环境安全。其作用机理是抑制真菌中甾醇的前体--羊毛甾醇或2,4-亚甲基二氢羊毛甾14位上的脱甲基化作用。丙硫菌唑中的杂质对其杀菌效果会产生一定的影响，需要对杂质进行定性分析后采取解决方案。
因此，急需一种操作简单，准确度高的丙硫菌唑中杂质的定性分析方法。
发明内容
为了解决现有丙硫菌唑中杂质的定性分析方法的问题，本发明提供一种丙硫菌唑中杂质的定性分析方法。
本发明提供了如下的技术方案：
一种丙硫菌唑中杂质的定性分析方法，包括如下步骤：
S1.取丙硫菌唑中杂质对照品，以乙腈为溶剂，配制丙硫菌唑中杂质对照品溶液；取丙硫菌唑原料药，以乙腈为溶剂，配制供试品溶液；以乙腈作为空白溶液；
S2.使用高效液相色谱仪和质谱检测器进行检测，色谱检测条件为：采用AgilentZORBAX Eclipse XDB-C18色谱柱，柱温为30-40℃，以水为流动相A，以乙腈水溶液为流动相B，流动相B中加入乙酸，流速为0.3-0.5mL/min；梯度洗脱程序为：0-1min，流动相B的体积百分数为20％；1-12min，流动相B的体积百分数由20％至30％；12-18min，流动相B的体积百分数为30％；18-18.1min，流动相B的体积百分数由30％至20％；18.1-23min，流动相B的体积百分数为20％；质谱检测条件为：离子模式为正离子模式，离子流数据采集范围为150-500Da，离子源温度为110-130℃，离子传输管温度为300-500℃，喷雾电压为2-4KV。
优选的,步骤S2中色谱检测条件的柱温为35℃，流速为0.4mL/min；质谱检测条件的离子流数据采集范围为350Da，离子源温度为120℃，离子传输管温度为400℃，喷雾电压为3KV。
优选的,步骤S2中乙腈水溶液中乙腈和水的体积比为7:3，加入乙酸的体积为乙腈水溶液的0.3％。
本发明的有益效果是：本发明采用Agilent ZORBAX Eclipse XDB-C18色谱柱，以十八烷基硅烷键合硅胶作为填充剂，利用水-乙腈水溶液作为流动相进行梯度洗脱，可以有效的分离丙硫菌唑中的杂质，采用质谱法对丙硫菌唑中的主要杂质峰进行定性分析，方便快捷，准确度高。
具体实施方式
实施例
一种丙硫菌唑中杂质的定性分析方法，包括如下步骤：
S1.取丙硫菌唑中杂质对照品，以乙腈为溶剂，配制丙硫菌唑中杂质对照品溶液；取丙硫菌唑原料药，以乙腈为溶剂，配制供试品溶液；以乙腈作为空白溶液；
S2.使用高效液相色谱仪和质谱检测器进行检测，色谱检测条件为：采用AgilentZORBAX Eclipse XDB-C18色谱柱，柱温为35℃，以水为流动相A，以乙腈水溶液为流动相B，流动相B中加入乙酸，流速为0.4mL/min；梯度洗脱程序为：0-1min，流动相B的体积百分数为20％；1-12min，流动相B的体积百分数由20％至30％；12-18min，流动相B的体积百分数为30％；18-18.1min，流动相B的体积百分数由30％至20％；18.1-23min，流动相B的体积百分数为20％；质谱检测条件为：离子模式为正离子模式，离子流数据采集范围为350Da，离子源温度为120℃，离子传输管温度为400℃，喷雾电压为3KV。
实验例
溶液配制见表1
表1
将六组试剂按照上述实验方法依次进行测定，其质谱解析结果如表2。
表2
根据反应原料和反应路线，得出杂质为2-(1-氯环丙基)-1-(2-氯苯基)-3-(1,2,4-三唑-1-基)-2-丙醇，结构式如下：
本技术方案通过能够快速准确的分析出丙硫菌唑中的杂质，通过分析表明，此分析方法的灵敏度和精确性均满足定形分析要求，能够为此类药物杂质的测定提供稳定的技术支持。
以上所述仅为本发明的优选实施例而已，并不用于限制本发明，尽管参照前述实施例对本发明进行了详细的说明，对于本领域的技术人员来说，其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (3)
1.一种丙硫菌唑中杂质的定性分析方法，其特征在于，包括如下步骤：
S1.取丙硫菌唑中杂质对照品，以乙腈为溶剂，配制丙硫菌唑中杂质对照品溶液；取丙硫菌唑原料药，以乙腈为溶剂，配制供试品溶液；以乙腈作为空白溶液；
S2.使用高效液相色谱仪和质谱检测器进行检测，色谱检测条件为：采用AgilentZORBAX Eclipse XDB-C18色谱柱，柱温为30-40℃，以水为流动相A，以乙腈水溶液为流动相B，流动相B中加入乙酸，流速为0.3-0.5mL/min；梯度洗脱程序为：0-1min，流动相B的体积百分数为20％；1-12min，流动相B的体积百分数由20％至30％；12-18min，流动相B的体积百分数为30％；18-18.1min，流动相B的体积百分数由30％至20％；18.1-23min，流动相B的体积百分数为20％；质谱检测条件为：离子模式为正离子模式，离子流数据采集范围为150-500Da，离子源温度为110-130℃，离子传输管温度为300-500℃，喷雾电压为2-4KV。
2.根据权利要求1所述的一种丙硫菌唑中杂质的定性分析方法，其特征在于,步骤S2中色谱检测条件的柱温为35℃，流速为0.4mL/min；质谱检测条件的离子流数据采集范围为350Da，离子源温度为120℃，离子传输管温度为400℃，喷雾电压为3KV。
3.根据权利要求1所述的一种丙硫菌唑中杂质的定性分析方法，其特征在于,步骤S2中乙腈水溶液中乙腈和水的体积比为7:3，加入乙酸的体积为乙腈水溶液的0.3％。
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| RENATA RAINA 等: "Determination of Azole Fungicides in Atmospheric Samples Collected in the Canadian Prairies by LC/MS/MS", 《JOURNAL OF AOA C INTERNATIONAL》 * |
| 刘淑杰 等: "丙硫菌唑的工艺改进", 《农药》 * |
| 史晓梅 等: "液相色谱-串联质谱法测定花生中丙硫菌唑及其脱硫代谢物", 《分析化学》 * |
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