主题：【讨论】卡波姆的残留溶剂

原文由 神话(fcqxqyslzx) 发表:

原文由 影子(hyheying) 发表:

原文由 神话(fcqxqyslzx) 发表:
我们来的料没有说，不知道是哪种，但苯的残留检验方法是一样的吧？

没有仔细比较过，你手头没有usp？

主要这个项目有问题，苯超，是用红色201单体为填料的填充柱

现在很少用填充柱了，用毛细管柱替代吧。

原文由 影子(hyheying) 发表:

原文由 tangtang(tangtang) 发表:

原文由 影子(hyheying) 发表:

原文由 tangtang(tangtang) 发表:

原文由 影子(hyheying) 发表:

原文由 tangtang(tangtang) 发表:
看看厂家的报告单，索取质量标准。

药典上已经有了。索取厂家的标准意义不大吧？

如果是中国药典的品种，厂家的注册标准有多于或严于药典的项目，要按注册标准来做的。

特别是残留溶剂，不同厂家不同工艺很可能检测的残留溶剂项目不一样。

USP的规定就不清楚了。

哦，忘记这事了。usp，ep与中国药典差不多，除了专论里指定的溶剂外还得遵守通则，也就是工艺特有溶剂

我们实际也是这么做的。反过来，就算厂家的注册标准里不包含药典品种正文项下的残留溶剂，我们也全做的。这样才算符合规定。

嗯，首先得符合药典标准，其实现在还有个更严的要求，工艺过程中可能产生的溶剂也需要进行残留控制，国内好像还没提这个

中国药典规定了的：

原文由 tangtang(tangtang) 发表:
中国药典规定了的：

我还真没注意到这里呢，谢谢糖糖，看来10版药典变化真的很大哦

934的：
Limit of benzene— Proceed as directed in the test for Limit of benzene under Carbomer 934P, except to use about 20 mg of Carbomer 934, accurately weighed, instead of about 1 g of Carbomer 934P, to prepare the Test solution. Calculate the percentage of benzene in the portion of Carbomer 934 taken by the formula:

10(C/W)(rU / rS)

in which C is the concentration, in µg per mL, of benzene in the Standard solution; W is the weight, in mg, of Carbomer 934 taken to prepare the Test solution; and rU and rS are the benzene peak responses obtained from the Test solution and the Standard solution, respectively: not more than 0.5% is found.

934P的：

Standard solution— Quantitatively dissolve an accurately weighed quantity of benzene in methanol to obtain a solution having a known concentration of about 0.2 mg per mL. Quantitatively dilute this solution with organic-free water (see Residual Solvents [img=12,20]mk:@MSITStore:E:\药典\USP\usp32_nf27_2009_roydan.chm::/pub/data/images/chars/lang.gif[/img]467[img=12,20]mk:@MSITStore:E:\药典\USP\usp32_nf27_2009_roydan.chm::/pub/data/images/chars/rang.gif[/img]) to obtain a solution having a known concentration of about 1.0 µg per mL.

Test solution— Transfer about 1 g of Carbomer 934P, accurately weighed, to a 100-mL volumetric flask. Add about 75 mL of sodium chloride solution (2 in 100), and mix by mechanical means until homogenous (usually about 30 minutes). Dilute with sodium chloride solution (2 in 100) to volume, and mix until homogenous (usually less than 1 minute). [note—This preparation must be analyzed within 3 hours of preparation.]

Chromatographic system (see Chromatography [img=12,20]mk:@MSITStore:E:\药典\USP\usp32_nf27_2009_roydan.chm::/pub/data/images/chars/lang.gif[/img]621[img=12,20]mk:@MSITStore:E:\药典\USP\usp32_nf27_2009_roydan.chm::/pub/data/images/chars/rang.gif[/img])— The gas chromatograph is equipped with a flame-ionization detector, a 0.53-mm × 30-m fused silica analytical column coated with a 3.0-µm G43 stationary phase, a 0.53-mm × 5-m silica guard column deactivated with phenylmethyl siloxane, and a splitless injection system. The carrier gas is helium flowing at a linear velocity of about 35 cm per second. The injection port and detector temperatures are maintained at 140[img=7,20]mk:@MSITStore:E:\药典\USP\usp32_nf27_2009_roydan.chm::/pub/data/images/chars/deg.gif[/img] and 260[img=7,20]mk:@MSITStore:E:\药典\USP\usp32_nf27_2009_roydan.chm::/pub/data/images/chars/deg.gif[/img], respectively. The column temperature is programmed according to the following steps: it is held at 40[img=7,20]mk:@MSITStore:E:\药典\USP\usp32_nf27_2009_roydan.chm::/pub/data/images/chars/deg.gif[/img] for 20 minutes, then increased rapidly to 240[img=7,20]mk:@MSITStore:E:\药典\USP\usp32_nf27_2009_roydan.chm::/pub/data/images/chars/deg.gif[/img], and maintained at 240[img=7,20]mk:@MSITStore:E:\药典\USP\usp32_nf27_2009_roydan.chm::/pub/data/images/chars/deg.gif[/img] for 20 minutes. Chromatograph the Standard solution, and record the responses as directed for Procedure: the relative standard deviation for replicate injections is not more than 15%.
Procedure— Separately inject equal volumes (about 1 µL) of the Standard solution and the Test solution into the chromatograph, record the chromatograms, and measure the responses for the benzene peaks. Calculate the percentage of benzene in the portion of Carbomer 934P taken by the formula:

10(C/W)(rU / rS)

in which C is the concentration, in µg per mL, of benzene in the Standard solution; W is the weight, in mg, of Carbomer 934P taken to prepare the Test solution; and rU and rS are the benzene peak responses obtained from the Test solution and the Standard solution, respectively: not more than 0.01% is found.

940：

Limit of benzene— Proceed as directed in the test for Limit of benzene under Carbomer 934P, except to use about 20 mg of Carbomer 940, accurately weighed, instead of about 1 g of Carbomer 934P, to prepare the Test solution. Calculate the percentage of benzene in the portion of Carbomer 940 taken by the formula:

10(C/W)(rU / rS)

in which C is the concentration, in µg per mL, of benzene in the Standard solution; W is the weight, in mg, of Carbomer 940 taken to prepare the Test solution; and rU and rS are the benzene peak responses obtained from the Test solution and the Standard solution, respectively: not more than 0.5% is found.

941：
Limit of benzene— Proceed as directed in the test for Limit of benzene under Carbomer 934P, except to use about 20 mg of Carbomer 941, accurately weighed, instead of about 1 g of Carbomer 934P, to prepare the Test solution. Calculate the percentage of benzene in the portion of Carbomer 941 taken by the formula:

10(C/W)(rU / rS)

in which C is the concentration, in µg per mL, of benzene in the Standard solution; W is the weight, in mg, of Carbomer 941 taken to prepare the Test solution; and rU and rS are the benzene peak responses obtained from the Test solution and the Standard solution, respectively: not more than 0.5% is found.

1342：
Limit of benzene— Proceed as directed in the test for Limit of benzene under Carbomer 934P, except to use about 50 mg of Carbomer 1342, accurately weighed, instead of about 1 g of Carbomer 934P, to prepare the Test solution. Calculate the percentage of benzene in the portion of Carbomer 1342 taken by the formula:

10(C/W)(rU / rS)

in which C is the concentration, in µg per mL, of benzene in the Standard solution; W is the weight, in mg, of Carbomer 1342 taken to prepare the Test solution; and rU and rS are the benzene peak responses obtained from the Test solution and the Standard solution, respectively: not more than 0.2% is found.

好象因为限度不同只是称样量上有所不同，没有很大的差别

原文由 影子(hyheying) 发表:

原文由 tangtang(tangtang) 发表:
中国药典规定了的：

我还真没注意到这里呢，谢谢糖糖，看来10版药典变化真的很大哦

有一个从严原则，基本上都可以套上。

尽量得到厂家的报告单，可以参考的

原文由 xiaowang268(xiaowang268) 发表:
尽量得到厂家的报告单，可以参考的

按照GMP要求，厂家的报告单是必须要有的

自己再检测，一般和检验单比对