血液净化医用吸附树脂中有机溶剂残留的GC-MS分析
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摘要
建立了气相色谱-质谱联用方法检测血液净化医用吸附树脂中苯、二乙苯、硝基苯和萘的分析方法。样品经三氯甲烷超声萃取,采用DB-624毛细管色谱柱分离,应用气相色谱-质谱选择离子监测模式定性定量检测,内标法定量。在各自的加标浓度下,平均加标回收率为89.7%～109.5%,相对标准偏差在7.5%～14%之间;方法的精密度均小于8.6%;线性范围为85.7～2 855μg/kg,相关系数均大于0.998 7。本方法操作简便,专属性及稳定性良好,结果可靠,经方法学验证,可用于血液净化医用吸附树脂中有机溶剂残留的测定。
The samples were extracted with trichlormethane and separated by DB-624 column,then determined by GC-MS in SIM mode.Recovery ranged from 89.7 to 109.5%,and the relative standard deviation was 7.5% —14%.The method precision was fine,RSD was lower than 8.6%.The linear range of 6 organic solvent residues was 85.7—2 855μg/kg,determination coefficients>0.998 7.The method is simple,rapid,reliable,good in specificity,stability and applicable for quantification of organic solvent residues in adsorption resin for blood purification.
The samples were extracted with trichlormethane and separated by DB-624 column,then determined by GC-MS in SIM mode.Recovery ranged from 89.7 to 109.5%,and the relative standard deviation was 7.5% —14%.The method precision was fine,RSD was lower than 8.6%.The linear range of 6 organic solvent residues was 85.7—2 855μg/kg,determination coefficients>0.998 7.The method is simple,rapid,reliable,good in specificity,stability and applicable for quantification of organic solvent residues in adsorption resin for blood purification.
引文
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[9]曾文雪,涂瑶生,王金钱,等.GC测定AB-8树脂中有机残留物间二乙烯苯和对二乙烯苯的含量[J].时珍国医国药,2013,24(4):802-803.
[10]刘忠文,洪育春,杨佳玲,等.气相色谱-质谱联用检测吸附树脂中溶剂残留物[J].解放军预防医学杂志,2010,28(3):176-179.
[2]马育.血液净化吸附剂研究进展[J].中国血液净化,2006,5(11):783-785.
[3]高文分,袁文娟,张启明,等.顶空气相色谱法测定三七总皂苷中有机溶剂残留量及大孔吸附树脂有机残留物[J].药物分析杂志,2007,27(3):460-463.
[4]郝或,刘虹,吴帅,等.顶空气相色谱法测定糖脂清片中大孔吸附树脂有机残留物[J].中成药,2009,31(9):1405-1408.
[5]廖淑彬,蔡韦炜,陈丹,等.顶空气相色谱法测定闽产三叶青地上部分抗炎镇痛提取物中大孔吸附树脂有机残留量[J].中国中医药科技,2016,23(6):688-690.
[6]王巧晗,杨小林,萧伟,等.木通皂苷D原料中有机溶剂残留量及大孔树脂有机残留物的测定[J].中国中药杂志,2015,40(10):1960-1964.
[7]梁文琳,谢达温,丁岗,等.顶空毛细管气相色谱法测定银杏叶片中大孔树脂残留物[J].世界科学技术-中医药现代化,2014,(8):1772-1776.
[8]王金钱,王焱,章军,等.固体树脂顶空进样GC法检测D-101系列大孔吸附树脂中3种低沸点有机溶剂残留量[J].中国实验方剂学杂志,2013,19(4):71-74.
[9]曾文雪,涂瑶生,王金钱,等.GC测定AB-8树脂中有机残留物间二乙烯苯和对二乙烯苯的含量[J].时珍国医国药,2013,24(4):802-803.
[10]刘忠文,洪育春,杨佳玲,等.气相色谱-质谱联用检测吸附树脂中溶剂残留物[J].解放军预防医学杂志,2010,28(3):176-179.