求一份EP 10.0的2.2.44. Total organic carbon in water for pharmaceutical use

ahah

求一份EP 10.0的2.2.44. Total organic carbon in water for pharmaceutical use，万分感激！

LanBo

2.2.44. TOTAL ORGANIC CARBON IN
WATER FOR PHARMACEUTICAL USE
Total organic carbon (TOC) determination is an indirect
measure of organic substances present in water for
pharmaceutical use. TOC determination can also be used
to monitor the performance of various operations in the
preparation of medicines.
A variety of acceptable methods is available for determining
TOC. Rather than prescribing a given method to be used,
this general chapter describes the procedures used to qualify
the chosen method and the interpretation of results in limit
tests. A standard solution is analysed at suitable intervals,
depending on the frequency of measurements; the solution
is prepared with a substance that is expected to be easily
oxidisable (for example, sucrose) at a concentration adjusted to
give an instrument response corresponding to the TOC limit
to be measured. The suitability of the system is determined by
analysis of a solution prepared with a substance expected to
be oxidisable with difficulty (for example, 1,4-benzoquinone).
The various types of apparatus used to measure TOC in
water for pharmaceutical use have in common the objective
of completely oxidising the organic molecules in the sample
water to produce carbon dioxide followed by measurement of
the amount of carbon dioxide produced, the result being used
to calculate the carbon concentration in the water.
The apparatus used must discriminate between organic and
inorganic carbon, the latter being present as carbonate. The
discrimination may be effected either by measuring the
inorganic carbon and subtracting it from the total carbon,
or by purging inorganic carbon from the sample before
oxidisation. Purging may also entrain organic molecules,
but such purgeable organic carbon is present in negligible
quantities in water for pharmaceutical use.
Apparatus. Use a calibrated instrument installed either on-line
or off-line. Verify the system suitability at suitable intervals as
described below. The apparatus must have a limit of detection
specified by the manufacturer of 0.05 mg or less of carbon
per litre.
TOC water. Use highly purified water complying with the
following specifications:
– conductivity: not greater than 1.0 μS·cm− 1 at 25 °C,
– total organic carbon: not greater than 0.1 mg/L.
Depending on the type of apparatus used, the content of
heavy metals and copper may be critical. The manufacturer’s
instructions should be followed.
Glassware preparation. Use glassware that has been
scrupulously cleaned by a method that will remove organic
matter. Use TOC water for the final rinse of glassware.
Standard solution. Dissolve sucrose R, dried at 105 °C for
3 h in TOC water to obtain a solution containing 1.19 mg of
sucrose per litre (0.50 mg of carbon per litre).
Test solution. Using all due care to avoid contamination,
collect water to be tested in an airtight container leaving
minimal head-space. Examine the water with minimum delay
to reduce contamination from the container and its closure.
System suitability solution. Dissolve 1,4-benzoquinone R in
TOC water to obtain a solution having a concentration of
0.75 mg of 1,4-benzoquinone per litre (0.50 mg of carbon
per litre)TOC water control. Use TOC water obtained at the same time
as that used to prepare the standard solution and the system
suitability solution.
Control solutions. In addition to the TOC water control,
prepare suitable blank solutions or other solutions needed
for establishing the baseline or for calibration adjustments
following the manufacturer’s instructions; run the appropriate
blanks to zero the instrument.
System suitability. Run the following solutions and record
the responses: TOC water (rw); standard solution (rs); system
suitability solution (rss). Calculate the percentage response
efficiency using the expression:
rss-rw
rs-rw           X100%
The system is suitable if the response efficiency is not less than
85 per cent and not more than 115 per cent of the theoretical
response.
Procedure. Run the test solution and record the response (ru).
The test solution complies with the test if ru is not greater than
rs – rw.
The method can also be applied using on-line instrumentation
that has been adequately calibrated and shown to have
acceptable system suitability. The location of instrumentation
must be chosen to ensure that the responses are representative
of the water used.

看饿了就点个宵

图               

jiangxiaojie123

附件中就是

ahah

LanBo 发表于 2021-8-23 11:00
2.2.44. TOTAL ORGANIC CARBON IN
WATER FOR PHARMACEUTICAL USE
Total organic carbon (TOC) determinat ...

谢谢~

ahah

jiangxiaojie123 发表于 2021-8-23 12:06
附件中就是

谢谢~

ahah

看饿了就点个宵 发表于 2021-8-23 11:03
图

谢谢~