关于USP中残留溶剂的测定

nn_kelun

实在是脱离这个行业太久了，弱弱的问几个问题： USP39-NF34_467 _RESIDUAL SOLVENTS.pdf (296.2 KB, 下载次数: 20)

2017-3-28 17:13 上传

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1)  第10页：关于一类和二类残留溶剂标准储备液的制备：我标黄的这些东东里面到底含哪些残留溶剂？订货号是多少？二类残留溶剂的Mixture A RS和Mixture A RS到底有啥区别呢？

Class 1 Standard Stock Solution—Transfer 1.0 mL of USP Class 1 Residual Solvents Mixture RS to a 100-mL volumetric flask, previously filled with about 9 mL of dimethyl sulfoxide, dilute with water to volume, and mix. Transfer 1.0mL of this solution to a 100-mL volumetric flask, previously filled with about 50 mL of water, dilute with water to volume, and mix. Transfer 10 mL of this solution to a 100-mL volumetric flask, previously filled with about 50 mL of water, dilute with water to volume, and mix.

Class 2 Standard Stock Solutions—Transfer 1.0 mL of USP Residual Solvents Class 2—Mixture A RS to a 100-mL volumetric flask, dilute with water to volume, and mix. This is Class 2 Standard Stock Solution A. Transfer 1.0 mL of USP Residual Solvents Class 2—Mixture B RS to a 100-mL volumetric flask, dilute with water to volume, and mix. This is Class 2 Standard Stock Solution B.

2)   第12页：方法C。为啥还要用一类标准溶液、一类系统适用性溶液来评价系统适用性？用户不能自己定义吗？

Chromatograph the Class 1 Standard Solution, the Class 1 System Suitability Solution, and the Class 2 Mixture A Standard Solution, and record the peak responses as directed for Procedure: the signal-to-noise ratio of 1,1,1-trichloroethane in the Class 1 Standard Solution is NLT 5; the signal-to-noise ratio of each peak in the Class 1 System Suitability Solution is NLT 3; and the resolution, R, between acetonitrile and methylene chloride in the Class 2 Mixture A Standard Solution is NLT 1.0.

yugijiang

没有看到你标黄的呀？

yugijiang

现在有这么个说法，采用467的方法，一类，二类溶剂残留方法只需要做方法确认，三类要做方法验证，供参考

nn_kelun

yugijiang 发表于 2017-3-28 20:15
没有看到你标黄的呀？

Word里标黄后粘过去，赶班车去了，没来得及检查，

nn_kelun

yugijiang 发表于 2017-3-28 20:16
现在有这么个说法，采用467的方法，一类，二类溶剂残留方法只需要做方法确认，三类要做方法验证，供参考

三类不是LOD吗？

一片红云

仅三类就LOD

yugijiang

最好还是做溶剂残留为好