液相色谱质谱联用检测血液和尿液中的琥珀胆碱及对标样的稳定性评价

Determination of succinycholine in the urine and plasma by LC/MS and stability evaluation of the reference materials

采用OasisR WCX固相萃取柱,用50%甲醇溶液洗脱杂质,并用1 mL甲酸-乙腈-水(1∶8∶1)溶液进行淋洗目标物。采用LC/MS/ESI检测其母离子为145.1,并选择115.5作为其定量离子。在尿液和血液中进行了回收率实验,测得其定量检测限分别为0.92ng/mL,1.89ng/mL(10倍S/N),方法的线性范围均在0.02～100μg/mL。并对标准物品在储存介质中的稳定性做了统计检验,测得10 d之内,1μg/mL琥珀胆碱标准样品在塑料容器中未检测到不稳定,储存稳定,而在玻璃容器中其降解几乎达90%。

The pretreatment process for succinycholine was as follows：using Oasis○R WCX as a SPE column（The sorbent is suitable for the extraction of the quaternary ammounium salts）,employing 50% methanol water solution to elute impurity,and using 1mL of 10% formic acid-80% acetonitrile water solution to elute the target compound.Because succinycholine has two positive charges,the ion at m/z =145.1 as the parent ion and the ion at m/z =115.5 for the quantitative ion were determined by LC/MS（ESI）.The method was evaluated by calculating the recovery with adding different amounts of succinycholine in the urine and blood.The experimental results showed that the limits of quantitation were 0.92 ng/mL in urine and 1.89 ng/mL in blood,respectively（at a signal to noise ratio of 10）,and the linear ranges in different matrixes were all between 0.02 μg/mLand 100 μg/mL.In the work,we also made the static evaluation for the reference materials by depositing 1μg/mL succinycholine in different mediums and measuring the respective responses during 10 days.The results showed that succinycholine was stable in the plastic,and it degradated obviously in the glass with degression of almost 90%.