CAJ | 학술논문

建立了气相色谱-三重四极杆质谱（GC-QQQ MS）同时测定生脉饮中17种邻苯二甲酸酯类化合物（ PAE）残留量的方法。样品经正己烷振摇提取后进行检测。采用 Agilent HP-5MS 毛细管色谱柱（30 m ×0.25 mm ×0.25μm）在程序升温条件下进行色谱分离；质谱以电子轰击（ EI）为电离方式，采用多反应监测（ MRM）模式进行监测。实验结果表明：17种 PAE 在0.5~20 mg / L 范围内呈线性关系，r 均大于0.99；平均加标回收率除邻苯二甲酸二甲酯（DMP）为51.9％、邻苯二甲酸二乙酯（ DEP）为77.2％外，其余15种为91.8％~117.2％，RSD（ n ＝6）为0.5％~5.4％。该方法操作简便，准确可靠，灵敏度高，专属性强，可用于生脉饮中邻苯二甲酸酯类化合物残留量的检测，以控制生脉饮的用药安全。
건립료기상색보-삼중사겁간질보（GC-QQQ MS）동시측정생맥음중17충린분이갑산지류화합물（ PAE）잔류량적방법。양품경정기완진요제취후진행검측。채용 Agilent HP-5MS 모세관색보주（30 m ×0.25 mm ×0.25μm）재정서승온조건하진행색보분리；질보이전자굉격（ EI）위전리방식，채용다반응감측（ MRM）모식진행감측。실험결과표명：17충 PAE 재0.5~20 mg / L 범위내정선성관계，r 균대우0.99；평균가표회수솔제린분이갑산이갑지（DMP）위51.9％、린분이갑산이을지（ DEP）위77.2％외，기여15충위91.8％~117.2％，RSD（ n ＝6）위0.5％~5.4％。해방법조작간편，준학가고，령민도고，전속성강，가용우생맥음중린분이갑산지류화합물잔류량적검측，이공제생맥음적용약안전。
Phthalate esters(PAEs)are commonly used for plastic products as plasticizer. Once taken in by human,PAEs will cause diseases,such as endocrine disorders,cancer,etc. Sheng-maiyin is a kind of Chinese medicine oral fluid whose packaging materials may include phthalate esters. If the phthalate esters migrated into the solution,it would lead to serious problem on the safety of drugs. In this study,a method of gas chromatography coupled to triple quadrupole mass spectrometry( GC-QQQ-MS) was developed for the simultaneous determination of 17 phthalate esters in Shengmaiyin samples. The samples were extracted with n-hexane by liquid-liquid extraction method before analysis. The separation was performed on an HP-5MS capillary column(30 m×0. 25 mm×0. 25 μm)with temperature programming. The MS / MS detection was performed under electron impact source(EI)in multi-reaction monitoring( MRM)mode. The good linear relationships were obtained in the range of 0. 5-20 mg / L for all the target analytes. The average recoveries of the 15 PAEs were in the range of 91. 8% - 117. 2% ,except dimethyl phthalate and diethyl phthalate which were about 51. 9% and 77. 2% ,respectively,and all the RSDs were in the range of 0. 5% - 5. 4% ( n = 6). The limits of detection ranged from 0. 04 to 16. 76 μg / L. The developed GC-MS method is simple,accurate,sensitive,proprietary,and can be applied in the detection of the phthalate ester residues in Shengmaiyin.