Simultaneous quantitation of hydrazine and acetylhydrazine in human plasma by high performance liquid chromatography-tandem mass spectrometry after derivatization with p-tolualdehyde
Simultaneous quantitation of hydrazine and acetylhydrazine in human plasma by high performance liquid chromatography-tandem mass spectrometry after derivatization with p-tolualdehyde
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对甲苯甲醛衍生化后高效液相色谱-串联质谱法同时定量人血浆中的肼和乙酰肼
DOI：
10.1016/j.jchromb.2017.08.036
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发表时间：
2017-09-15
影响因子：
3
通讯作者：
Jiang, Yuyang
中科院分区：
文献类型：
--
作者：
Song, Lu;Gao, Dan;Jiang, Yuyang
基于对甲苯甲醛衍生化策略，建立了一种同时测定人血浆中肼和乙酰肼的高效液相色谱-串联质谱法。超声处理40min即可实现衍生化反应。采用C-18色谱柱进行梯度洗脱，实现了衍生化产物的良好分离。两种肼类化合物的优化质量跃迁离子对(m/z)分别为m/z 237.1>；>；>；119.9和m/z 176.9>；>；>；117.8。肼的检出限和定量限分别为0.002和0.005 ng mL(-1)。乙酰肼分别为0.03和0.05 ng·mL~(-1)。联氨和乙酰肼的线性范围分别为0.005-50ngmL(-1)和0.005-500ngmL(-1)，R-2>0.999。加标回收率为95.38-108.12%，相对标准偏差为1.24-14.89%。该方法已成功应用于30例异烟肼治疗肺结核患者的临床血浆标本检测。肼和乙酰肼的浓度分别为0.04~1.99ngmL(-1)和0.06~142.43 ngmL(-1)。结果表明，我们建立的方法具有检测复杂生物样品中肼类毒物的潜力。该方法对临床药物治疗具有重要意义。
A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed for simultaneous quantitative analysis of hydrazine and acetylhydrazine in human plasma based on the strategy of p-tolualdehyde derivatization. The derivatization reactions were easily realized by ultrasonic manipulation for 40 min. Good separation of the derivatization products was achieved using a C-18 column by gradient elution. The optimized mass transition ion-pairs (m/z) monitored for the two hydrazine derivatives were m/z 237.1 >> > 119.9 and m/z 176.9 >> > 117.8, respectively. The limit of detection (LOD) and limit of quantification (LOQ) for hydrazine were 0.002 and 0.005 ng mL(-1) separately. And they were 0.03 and 0.05 ng mL(-1) for acetylhydrazine, respectively. The linear range was 0.005-50 ng mL(-1) for hydrazine and 0.05-500 ng mL(-1) for acetylhydrazine with R-2 greater than 0.999. The recovery range was determined to be 95.38-108.12% with the relative standard deviation (RSD) in the range of 1.24-14.89%. The method was successfully applied to detect 30 clinical plasma samples of pulmonary tuberculosis patients treated with isoniazid. The concentrations were from 0.04-1.99 ng mL(-1) for hydrazine and 0.06-142.43 ng mL(-1) for acetylhydrazine. The results indicated that our developed method had the potential for the detection of hydrazine toxicology in complex biological samples. Furthermore, the method has an important significance to clinical treatment with drugs.