原文由 神话(fcqxqyslzx) 发表:
卡波姆的残留溶剂,美国药典USP32 怎么说的
药典上很多,神话想要哪一种呢:
好象苯的残留是必须检的,其它溶剂应该是根据工艺情况按通则进行。
Limit of benzene— 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.