【摘 要】
：
采用气相色谱-串联质谱法(GC-MS/MS),建立了螺旋霉素原料药中N-亚硝基二甲胺(NDMA)含量的检测方法.样品的制备使用液液萃取法,先将螺旋霉素溶于硫酸溶液,再用二氯甲烷萃取得
【机 构】
：
天方药业有限公司河南省心脑血管药物重点实验室,驻马店463000
论文部分内容阅读
采用气相色谱-串联质谱法(GC-MS/MS),建立了螺旋霉素原料药中N-亚硝基二甲胺(NDMA)含量的检测方法.样品的制备使用液液萃取法,先将螺旋霉素溶于硫酸溶液,再用二氯甲烷萃取得到待测液.质谱检测使用多反应扫描模式,定量离子对为74.0→4.0,定性离子对为74.0→42.0.在0.25～50 μg/L范围内的NDMA质量浓度与响应呈现良好线性关系,相关系数为0.99998,仪器检测限和定量限分别为0.1260和0.3819 μg/L.低、中和高3个水平下的硫酸溶液加标回收率在100.20％ ～ 103.07％,相对标准偏差(RSD)在0.27％ ～0.72％,螺旋霉素硫酸溶液的加标回收率在103.23％ ～ 107.87％,RSD在0.56％ ～0.64％.方法 重复性检测结果RSD为4.25％.螺旋霉素加酸溶解后放置0、2、4和6h再萃取,检测结果RSD为2.86％.待测溶液放置0～24h的峰面积RSD为3.14％,NDMA标准品工作液放置0～24h的峰面积RSD为3.42％.使用该方法在螺旋霉素原料药中检出的NDMA含量均未超标.
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