CN114878736B - 一种联苯肼酯中杂质的测定方法 - Google Patents
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Abstract
本发明涉及农药检测技术领域，特别是涉及一种联苯肼酯中杂质的测定方法，包括如下步骤：S1、分别称取标样联苯肼酯杂质，再分别用甲醇溶解并配制成对应的标样溶液；S2、称取联苯肼酯原药，利用甲醇溶解并配制成样品溶液；S3、利用液质联用仪分别测定标样溶液和样品溶液；其中，联苯肼酯杂质I为3‑氨基‑4‑甲氧基联苯，联苯肼酯杂质Ⅱ为2‑(4‑甲氧基‑3‑(1,1‑二苯基)‑3‑基)偶氮羧酸异丙酯。本发明采用液质联用仪对联苯肼酯原药可能存在的副产物及杂质进行检测，将原药通过液相色谱分离，再利用质谱仪进行分析比对，能够准确地鉴定和分析农药联苯肼酯中存在的杂质，进而避免杂质影响联苯肼酯质量。
Description
技术领域
本发明涉及农药检测技术领域，特别是涉及一种联苯肼酯中杂质的测定方法。
背景技术
联苯肼酯(分子式C17H20N2O3)又称3-(4-甲氧基联苯基-3-基)肼基甲酸异丙酯，是一种新型选择性叶面喷雾用联苯肼类杀螨剂，其纯品外观为白色固体结晶，其作用机理为对螨类的线粒体电子传递链复合体III抑制剂的独特作用，主要用于防治苹果红蜘蛛、二斑叶螨、McDaniel螨、观赏植物的二斑叶螨和Lewis螨。联苯肼酯对螨的各个生活阶段有效，具有杀卵活性和对成螨的击倒活性(48～72h)，且持效期在14天左右，持效期长，推荐使用剂量范围内对作物安全，对寄生蜂、捕食螨、草蛉低风险。
由于农药联苯肼酯并非完全纯品，原药中通常存在杂质，杂质容易影响联苯肼酯质量，目前行业内暂未对农药实际生产中可能带来的副产物以及杂质确定检测、分析方法，因此无法进行对农药联苯肼酯的杂质进行准确检测。
发明内容
本发明的目的在于提供一种联苯肼酯中杂质的测定方法，以解决上述背景技术中提出的问题。
本发明是通过以下技术方案实现的：
一种联苯肼酯中杂质的测定方法，包括如下步骤：
S1、分别称取标样联苯肼酯杂质I和标样联苯肼酯杂质Ⅱ，再分别用甲醇溶解并配制成对应的标样溶液1和标样溶液2；
S2、称取联苯肼酯原药，利用甲醇溶解并配制成样品溶液；
S3、利用液质联用仪分别测定标样溶液1、标样溶液2和样品溶液；
其中，联苯肼酯杂质I为3-氨基-4-甲氧基联苯，联苯肼酯杂质Ⅱ为2-(4-甲氧基-3-(1,1-二苯基)-3-基)偶氮羧酸异丙酯，其结构式分别为：
作为本发明的进一步方案，液质联用仪中，液相色谱柱选用Agilent EclipseXDB-C18 2.1×150mm，5μm，其色谱条件设置如下：柱温设置为35℃，流速为0.3mL/min，运行时间为25min。
优选的，采用分流进样的形式，每次进样量为5.0μL。
优选的，采用超纯水和甲醇进行梯度洗脱，其中，联苯肼酯杂质I的保留时间为6.7min，联苯肼酯杂质Ⅱ的保留时间为12.3min。
作为本发明的进一步方案，液质联用仪中，质谱检测选用ESI离子源，其质谱条件设置如下。
| 离子源 | ESI | 离子化方式 | 正离子模式 |
| 扫描模式 | SCAN | 扫描范围 | m/z 120-500 |
| Capillary(KV) | 3.50 | Cone(V) | 30 |
| Extractor(V) | 3 | RF Len(V) | 0.3 |
| Source Temp(℃) | 120 | Desolvation Temp(℃) | 400 |
| Desolvation(L/Hour) | 400 | Cone(L/Hour) | 50 |
| LM Resolution | 15.0 | HM Resolution | 15.0 |
| Ion Energy | 0.5 | Multiplier | 650 |
优选的，所述标样联苯肼酯杂质I和标样联苯肼酯杂质Ⅱ的纯度均为94.0～99.0％。
与现有技术相比，本发明的有益效果是：
本发明采用液质联用仪对联苯肼酯原药可能存在的副产物及杂质进行检测，将原药通过液相色谱分离，再利用质谱仪高质量分辨、高灵敏等特点，对化合物离子及二级质谱的离子碎片进行分析比对，能够准确地鉴定农药联苯肼酯中含有的杂质信息，进而对原药中存在的杂质进行分析，避免杂质影响联苯肼酯质量。
附图说明
为了更清楚地说明本发明实施例的技术方案，下面将对实施例描述所需要使用的附图作简单地介绍，对于本领域普通技术人员来讲，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为本发明联苯肼酯原药的总离子流图；
图2为本发明联苯肼酯原药中杂质的质谱图；
图3为本发明标样联苯肼酯杂质I的总离子流图；
图4为本发明标样联苯肼酯杂质I的质谱图；
图5为本发明标样联苯肼酯杂质Ⅱ的总离子流图；
图6为本发明标样联苯肼酯杂质Ⅱ的质谱图。
具体实施方式
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。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其它实施例，都属于本发明保护的范围。
若如无特别说明，实施例中所使用的材料均可容易地从商业公司获取，所用甲醇为色谱纯试剂(批号16095070，美国Tidea公司)。在相同的操作条件下，联苯肼酯原药中杂质I、杂质Ⅱ与标样杂质I、标样杂质Ⅱ的保留时间相同，质谱各质荷比相对峰强度也一致。
本实施例提供了一种联苯肼酯中杂质的测定方法，包括如下步骤：
S1、称取3mg标样联苯肼酯杂质I(纯度为99.0％)于25mL容量瓶A中，称取3mg标样联苯肼酯杂质Ⅱ(纯度为94.0％)于25mL容量瓶B中，分别用甲醇均匀溶解、配制并定容，得到标样溶液1和标样溶液2；
S2、称取50mg联苯肼酯原药于25mL容量瓶C中，利用甲醇溶解并配制成样品溶液；
S3、利用液质联用仪分别测定标样溶液1、标样溶液2和样品溶液；
其中，液相色谱柱选用Agilent Eclipse XDB-C18 2.1×150mm，5μm，测定时采用分流进样的形式，每次进样量为5.0μL，其色谱条件设置如下：柱温设置为35℃，流速为0.3mL/min，运行时间为25min。
液相色谱分离杂质时采用超纯水和甲醇进行梯度洗脱，梯度洗脱程序如下：
| 时间(min) | 水(％) | 甲醇(％) | 流速(mL/min) | Curve |
| 0 | 45 | 55 | 0.30 | 1 |
| 10.0 | 15 | 85 | 0.30 | 6 |
| 15.0 | 15 | 85 | 0.30 | 6 |
| 15.5 | 45 | 55 | 0.30 | 6 |
| 25.0 | 45 | 55 | 0.30 | 6 |
质谱检测选用ESI离子源，其质谱条件设置如下：
| 离子源 | ESI | 离子化方式 | 正离子模式 |
| 扫描模式 | SCAN | 扫描范围 | m/z 120-500 |
| Capillary(KV) | 3.50 | Cone(V) | 30 |
| Extractor(V) | 3 | RF Len(V) | 0.3 |
| Source Temp(℃) | 120 | Desolvation Temp(℃) | 400 |
| Desolvation(L/Hour) | 400 | Cone(L/Hour) | 50 |
| LM Resolution | 15.0 | HM Resolution | 15.0 |
| Ion Energy | 0.5 | Multiplier | 650 |
根据上述检测方法，分别测定杂质混合参照物溶液及样品溶液，得到对应的总离子流图及质谱图。
如附图1-4所示，保留时间6.7min的组分为杂质I，联苯肼酯原药中杂质I质谱解析如下表所示，由反应路线及杂质谱图的碎片峰质荷比可知，杂质I为3-氨基-4-甲氧基联苯，结构式为：
| 编号 | 联苯肼酯原药 | 杂质标样I |
| 分子加氢峰m/z | 200.47 | 200.46 |
如附图1-2、5-6所示，保留时间12.3min的组分为杂质Ⅱ，联苯肼酯原药中杂质Ⅱ质谱解析如下表所示，由反应路线及杂质谱图的碎片峰质荷比可知，杂质Ⅱ为2-(4-甲氧基-3-(1,1-二苯基)-3-基)偶氮羧酸异丙酯，结构式为：
| 编号 | 联苯肼酯原药 | 杂质标样I |
| 分子加氢峰m/z | 299.43 | 299.43 |
| 分子加钠峰m/z | 321.44 | 321.43 |
本发明采用液质联用仪对联苯肼酯原药可能存在的副产物及杂质进行检测，将原药通过液相色谱分离，再利用质谱仪进行分析比对，能够准确地鉴定和分析农药联苯肼酯中存在的杂质，进而避免杂质影响联苯肼酯质量。
以上公开的本发明优选实施例只是用于帮助阐述本发明。优选实施例并没有详尽叙述所有的细节，也不限制该发明仅为所述的具体实施方式。显然，根据本说明书的内容，可作很多的修改和变化。本说明书选取并具体描述这些实施例，是为了更好地解释本发明的原理和实际应用，从而使所属技术领域技术人员能很好地理解和利用本发明。本发明仅受权利要求书及其全部范围和等效物的限制。
Claims (4)
1.一种联苯肼酯中杂质的测定方法，其特征在于，包括如下步骤：
S1、分别称取标样联苯肼酯杂质I和标样联苯肼酯杂质Ⅱ，再分别用甲醇溶解并配制成对应的标样溶液1和标样溶液2；
S2、称取联苯肼酯原药，利用甲醇溶解并配制成样品溶液；
S3、利用液质联用仪分别测定标样溶液1、标样溶液2和样品溶液；
其中，联苯肼酯杂质I为3-氨基-4-甲氧基联苯，联苯肼酯杂质Ⅱ为2 - (4 -甲氧基- 3-(1, 1-二苯基)-3-基)偶氮羧酸异丙酯，其结构式分别为：
I
Ⅱ
液质联用仪中，液相色谱柱选用Agilent Eclipse XDB-C18 2.1×150 mm，5μm，其色谱条件设置如下：柱温设置为35℃，流速为0.3 mL/min，运行时间为25min；
液质联用仪中，质谱检测选用ESI离子源，离子源温度设置为120℃，离子化方式设置为正离子模式，质谱的扫描范围为120~500amu；
液质联用仪梯度洗脱程序如下：
。
2.根据权利要求1所述的一种联苯肼酯中杂质的测定方法，其特征在于，采用分流进样的形式，每次进样量为5.0μL。
3.根据权利要求1所述的一种联苯肼酯中杂质的测定方法，其特征在于，采用超纯水和甲醇进行梯度洗脱，其中，联苯肼酯杂质I的保留时间为6.7min，联苯肼酯杂质Ⅱ的保留时间为12.3min。
4.根据权利要求1所述的一种联苯肼酯中杂质的测定方法，其特征在于，所述标样联苯肼酯杂质I和标样联苯肼酯杂质Ⅱ的纯度均为94.0~99.0%。
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| CN102344395A (zh) * | 2011-07-28 | 2012-02-08 | 同济大学 | 一种联苯肼酯的合成方法 |
| CN109254099A (zh) * | 2018-11-30 | 2019-01-22 | 中国测试技术研究院 | 农药制剂中非登记成分的气相色谱-质谱快速测定方法 |
| CN109988084A (zh) * | 2019-04-23 | 2019-07-09 | 绍兴上虞新银邦生化有限公司 | 一种联苯肼酯合成方法 |
| CN110381738A (zh) * | 2016-10-14 | 2019-10-25 | 勃林格殷格翰动物保健美国公司 | 农药的和杀寄生物的乙烯基异噁唑啉化合物 |
| WO2020117688A2 (en) * | 2018-12-04 | 2020-06-11 | Orochem Technologies Inc. | Process for purifying tetrahydrocannabinol using a chromatographic stationary phase |
| CN113933435A (zh) * | 2021-10-27 | 2022-01-14 | 湖南文谱检测技术研究有限公司 | 一种快速检测柑橘中联苯肼酯及其代谢物残留量的超高效液相色谱串联质谱法 |
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| CA3089347C (en) * | 2018-01-23 | 2023-06-27 | Perkinelmer Health Sciences, Inc. | Triple quadrupole mass spectrometers configured to detect mrm transitions of pesticide residues |
| US11181512B2 (en) * | 2018-04-16 | 2021-11-23 | Chinese Academy Of Inspection And Quarantine | Electronic ID database and detection method for pesticide compounds in edible Agro-products based on GC-Q-Orbitrap |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102344395A (zh) * | 2011-07-28 | 2012-02-08 | 同济大学 | 一种联苯肼酯的合成方法 |
| CN110381738A (zh) * | 2016-10-14 | 2019-10-25 | 勃林格殷格翰动物保健美国公司 | 农药的和杀寄生物的乙烯基异噁唑啉化合物 |
| CN109254099A (zh) * | 2018-11-30 | 2019-01-22 | 中国测试技术研究院 | 农药制剂中非登记成分的气相色谱-质谱快速测定方法 |
| WO2020117688A2 (en) * | 2018-12-04 | 2020-06-11 | Orochem Technologies Inc. | Process for purifying tetrahydrocannabinol using a chromatographic stationary phase |
| CN109988084A (zh) * | 2019-04-23 | 2019-07-09 | 绍兴上虞新银邦生化有限公司 | 一种联苯肼酯合成方法 |
| CN113933435A (zh) * | 2021-10-27 | 2022-01-14 | 湖南文谱检测技术研究有限公司 | 一种快速检测柑橘中联苯肼酯及其代谢物残留量的超高效液相色谱串联质谱法 |
Non-Patent Citations (3)
| Title |
|---|
| HPLC-MS/MS法同时测定水中联苯肼酯和乙螨唑残留量;魏杰 等;食品安全导刊;第76-78页 * |
| 新农药联苯肼酯的光化学降解;戴魏 等;环境化学;第33卷(第2期);第334-340页 * |
| 联苯肼酯43%悬浮剂的高效液相色谱分析;肖峥 等;农药科学与管理;第31卷(第08期);第40-42页 * |
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