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British Pharmacopoeia 2016

Volume IV

Page 395

2016 St. John’s Wort IV-387


50 mL with water. To 20 mL of this solution add 8 mL of a

freshly prepared 1.0% w/v solution of sodium nitrite, allow to

stand for 15 minutes, add 12 mL of 5m ammonia, dilute to

50 mL with water and measure the absorbance of a 4-cm layer

of the resulting solution at the maximum at 442 nm,

Appendix IT B, using in the reference cell a solution prepared

in the same manner and at the same time but using 8 mL of

water in place of the solution of sodium nitrite. Calculate the

content of C,;7H;,9NO3 from a calibration curve prepared

using quantities of 2, 4, 6 and 8 mL of a 0.008% w/v

solution of anhydrous morphine in 0.1m hydrochloric acid, each

diluted to 20 mL with 0.1m hydrochloric acid and using the

method described above beginning at the words ‘add 8 mL

.... Determine the weight per mL of the linctus,

and calculate the content of C,7H);)9NO3,





St. John’

Hypericum

(Ph. Eur. monograph

Preparation

St. John’s Wort Dry Extre

Ph Eur

DEFINITION
Whole or fragmented, dried flowering

perforatum L., harvested during flowering





Content é

Minimum 0.08 per cent of total hypericins, express

hypericin (C39H, 608; M, 504.4) (dried drug).

IDENTIFICATION

A. The branched and bare stem shows 2 more or less

prominent longitudinal ridges. The leaves are opposite,

sessile, exstipulate, oblong-oval and 15-30 mm long; prese

on the leaf margins are glands which appear as black dots

and over all the surface of the leaves many small, strongly

translucent excretory glands which are visible in transmitted

light. The flowers are regular and form corymbose clusters at

the apex of the stem. They have 5 green, acute sepals, with

black secretory glands on the margins; 5 orange-yellow

petals, also with black secretory glands on the margins;

3 staminal blades, each divided into many orange-yellow

stamens and 3 carpels surmounted by red styles.



The drug may also show the following: immature and ripe

fruits and seeds. Immature fruits are green or yellowish, seeds

are whitish. Occasional ripe fruits may be present; these are

dry trilocular capsules containing numerous seeds, brown,

broad or small-ovate, 5-10 mm long, with broad linear or

punctiform glands, irregularly striated ducts, conducting

secretions. Ripe seeds are 1-1.3 mm long, cylindrical or

trigonous, shortly pointed at both ends, brown or almost

black, minutely pitted longitudinally.

B. Microscopic examination (2.8.23). The powder is

greenish-yellow. Examine under a microscope using chloral

hydrate solution R. The powder shows the following diagnostic

characters (Figure 1438.-1): fragments of the leaf epidermis

[A, B] or stems [H] with paracytic [Ab, Ha], anisocytic [Ac,

Bb, Hb] or anomocytic [Ae] stomata (2.8.3); fragments of

the leaf epidermis often accompanied by palisade

parenchyma [Ad, Bc]; polygonal cells of the upper epidermis

with thickened and beaded walls [Ba]; more or less sinuous,

thin-walled cells of the lower epidermis [Aa]; fragments of

the leaf and sepal [E] with large, red-pigmented oil glands

[Ea] associated with palisade parenchyma [Eb] and small

vessels [Ec]; elongated cells of fragments of the petal

epidermis with straight or wavy anticlinal walls [J];

vessels [D] with reticulate or pitted walls [Da] and groups of

thick-walled fibres [Db]; fragments of the central parenchyma

of the stems [K] with lignified and pitted rectangular

cells [Ka] sometimes associated with vessels [Kb]; fragments

of the anthers [F] showing the central part consisting of small

cells containing cluster crystals of calcium oxalate [Fb] and

cells from the fibrous layer [Fa]; fragments of the staminal

filament with elongated, thin-walled cells with a striated

cuticle [C]; numerous pollen grains with 3 germinal pores

and a smooth exine, occurring singly [G] or in dense groups.


























herbal drug of St. Ff

C. Thin-layer chroma

10 min and filter.

Reference solution Dissolve 5 mg of

rutin Rin methanol R, then dilute to

solvent.

Plate TLC sihca gel plate R.

Mobile phase anhydrous formic acid R, water R, ethyl acetate R

(6:9:90 V/V/V).

Apphcation 10 uwL of the test solution and 5 uL of the

reference solution, as bands of 10 mm.

and 5 mg of

h the same

Development Over a path of 10 cm.

Drying At 100-105 °C for 10 min.

Detection Treat with a 10 g/L solution of diphenylboric acid

aminoethyl ester R in methanol R and then with a 50 g/L

solution of macrogol 400 R in methanol R. After about 30 min,

examine in ultraviolet light at 365 nm.

Results The chromatogram obtained with the reference

solution shows in the lower third a zone due to rutin and

Page 396

IV-388 St. John’s Wort Preparations 2016


above it a zone due to hyperoside, both with yellow-orange

fluorescence. The chromatogram obtained with the test

solution shows in the lower third 2 reddish-orange

fluorescent zones due to rutin and hyperoside, and in the

lower part of the upper third a zone due to pseudohypericin

and above it a zone due to hypericin, both with red

fluorescence. Other yellow or blue fluorescent zones are

visible.

TESTS

Foreign matter (2.8. 2)

Maximum 3 per cent of stems with a diameter greater than

5 mm and maximum 2 per cent of other foreign matter.

Loss ona (2.2.32)






















ttomed flask, introduce

0.800 g of the powdered ag (500) (2.9.12), 60 mL

of a mixture of 20 volumes

er for 30 min.

mt the Supernatant into
a 250 mL flask. Take up the residue witt

mixture of 20 volumes of water R and 80

Take up the residue with 15 mL of methanol R with tt
of ultrasound and transfer to a 25 mL measuring flask.

the 250 mL flask with methanol R and dilute to 25.0 mL w

the same solvent. Centrifuge again, filter 10 mL through a

syringe filter (0.2 um). Discard the first 2 millilitres of the

filtrate. Introduce 5.0 mL of the filtrate into a measuring

flask and dilute to 25.0 mL with methanol R.

Compensation liquid methanol R.

Measure the absorbance (2.2.25) at 590 nm of the test

solution, by comparison with the compensation liquid.

Calculate the percentage content of total hypericins,

expressed as hypericin, using the following expression:

A x 125

m x 870

. taking the specific absorbance of hypericin to be 870.

= absorbance at 590 nm;

= mass of the herbal drug to be examined, in grams.S
A
D

Ph Eur

Kk%
Quantified St. John’s Wort Dry >
Extract
(Ph, Eur. monograph 1874)

Ph Eur

DEFINITION

Quantified dry extract obtained from St. Fohn’s wort (1438).

%

xy



Content

— total hypericins, expressed as hypericin (C39H 60g; M,

504.5): 0.10 per cent to 0.30 per cent (anhydrous

extract);




















— flavonoids, expressed as rutin (C27H390163M, 610.5):

minimum 6.0 per cent (anhydrous extract);

— hyperforin (C35H5,0,; M, 536.8): maximum 6.0 per cent

(anhydrous extract) and not more than the content stated

on the label.

PRODUCTION

The extract is produced from the herbal drug by a suitable

procedure using ethanol (50-80 per cent V/V) or methanol

(50-80 per cent V/V).

CHARACTERS

Appearance

Brownish-grey powder.

IDENTIFICATION

Thin-layer chromatography (2.2.27).

Test solution Disperse 0.25 g of the extract to be examined in

5 mL of methanol R.

Reference solution Dissolve 5 mg of rutin R and 5 mg of

hyperoside R in methanol R and dilute to 10 mL with the same

solvent.

Plate TLC silica gel plate R (5-40 uum) [or TLC silica gel

plate R (2-10 um)].

Mobile phase anhydrous formic acid R, water R, ethyl acetate R

(6:9:90 V/V/V).

Application 10 wL [or 5 pL] as bands of 10 mm [or 8 mm].

Development Over a path of 10 cm [or 7.5 cm].

Drying At 100-105 °C for 10 min.

Detection Treat with a 10 g/L solution of diphenylboric acid

aminoethyl ester R in methanol R and then with a 50 g/L

solution of macrogol 400 R in methanol R. Examine after

about 30 min in ultraviolet light at 365 nm.

isSee below the sequence of zones present in the

grams obtained with the reference solution and the

n. Furthermore, other fluorescent zones may be

the chromatogram obtained with the test solution.



Top of the plate


A yellowish-orange fluorescent
zone

2 red fluorescent zones (hypericin
and pseudohypericin)

Hyperoside: a yellowish-orange
fluorescent zone zone (hyperoside}

Yellow and bluepéssibl
superimposed fluoresg¢grit zones
A yellowish-orange fluorescent
zone (rutin)

Rutin: a yellowish-orange
fluorescent zone


Reference solution Test solution
TESTS

Water (2.5.12)

Maximum 4.0 per cent, determined on 0.5 g.

ASSAY

Total hypericins

Liquid chromatography (2.2.29).

Test solution Dissolve 70.0 mg of the extract to be examined

in 25.0 mL of methanol R. Sonicate and centrifuge the

Page 789

2016 Surgical Materials IV-781


other end held in the left hand, passing one end over the

suture and through the loop so formed (see Figure 0324.-1)

and pulling the knot tight. For stainless steel sutures gauges

3.5 and above, the minimum breaking load is determined on

a straight pull. Carry out the test on 5 sutures. Submit

sutures of length greater than 75 cm to 2 measurements and

shorter sutures to 1 measurement. Determine the breaking

load using a suitable tensilometer. The apparatus has

2 clamps for holding the suture, 1 of which is mobile and is

driven at a constant rate of 30 cm/min. The clamps are

designed so that the suture being tested can be attached

without any possibility of slipping. At the beginning of the

test the length of suture between the clamps is 12.5 cm to

20 cm and the knot is midway between the clamps. Set the



he suture breaks in a clamp or within 1 cm of
is.<iscarded and the test repeated on another
































d, is equal to or greater than the value
Eable 0324.-1 and no value is less than

Figure 0324.-1. — Simple knot

Needle attachment

If the sutures are supplied with an eyeless needle attached

that is not stated to be detachable, they comply with the test

for needle attachment. Carry out the test on 5 sutures. Use a

suitable tensilometer, such as that described for the

determination of the minimum breaking load. Fix the needle

and suture (without knot) in the clamps of the apparatus in

such a way that the swaged part of the needle is completely

free of the clamp and in line with the direction of pull on the

suture. Set the mobile clamp in motion and note the force

required to break the suture or to detach it from the needle.

The average of the 5 determinations and all individual values

are not less than the respective values given in Table 0324.-2

for the gauge number concerned. If not more than

1 individual value fails to meet the individual requirement,

repeat the test on an additional 10 sutures. The attachment

complies with the test if none of these 10 values is less than

the individual value in Table 0324.-2 for the gauge number

concerned.

Extractable colour

Sutures that are dyed and intended to remain so during use

comply with the test for extractable colour. Place 0.25 g of

the suture to be examined in a conical flask, add 25.0 mL of

water R and cover the mouth of the flask with a short-

stemmed funnel. Boil for 15 min, cool and adjust to the

original volume with water R. Depending on the colour of the

suture, prepare the appropriate reference solution as

described in Table 0324.-3 using the primary colour

solutions (2.2.2).

The test solution is not more intensely coloured than the

appropriate reference solution.

Monomer and oligomers

Polyamide-6 suture additionally complies with the following

test for monomer and oligomers. In a continuous-extraction

apparatus, treat 1.00 g with 30 mL of methanol R at a rate of

at least 3 extractions per hour for 7 h. Evaporate the extract

to dryness, dry the residue at 110 °C for 10 min, allow to

cool in a desiccator and weigh. The residue weighs not more

than 20 mg (2 per cent).

STORAGE (PACKAGING)

Sterile non-absorbable sutures are presented in a suitable

sachet that maintains sterility and allows the withdrawal and

use of a suture in aseptic conditions. They may be stored dry

or in a preserving liquid to which an antimicrobial agent but

no antibiotic may be added.

Sterile non-absorbable sutures are intended to be used only

on the occasion when the sachet is first opened.

Sutures in their individual sachets (primary packaging) are

kept in a protective cover (box) which maintains the physical

and mechanical properties until the time of use.

The application of appropriate harmonised standards for

packaging of medical devices shall be considered in addition.

Table 0324.-2. - Minimum strengths of needle attachment




Gauge number Mean value Individual value
(newtons) (newtons)

0.4 0.50 0.25

0.5 0.80 0.40

0.7 1.7 0.80

2.3 1.1

5 4.5 2.3

6.8 3.4

9.0 4.5

11.0 4.5

15.0 4.5

6.0

5 7.0

6

7

8

9

10


Table 0324.-3. - Colour reference solutions






Colour of Composition of reference solution
strand (parts by volume)

Red Yellow Blue Water R
primary primary primary
solution solution solution

Yellow-brown 0.2 1.2 - 8.6

Pink-red 1.0 : - 9.0

Green-blue 2.0 8.0

Violet 1.6 - 8.4

Page 790

IV-782 Surgical Materials 2016


LABELLING

Reference may be made to the appropriate harmonised

standards for the labelling of medical devices.

The details strictly necessary for the user to identify the

product properly are indicated on or in each sachet (primary

packaging) and on the protective cover (box) and include at

least:

— gauge number,

— length, in centimetres or metres,

— if appropriate, that the needle is detachable,

— name of the product,

— intended use (surgical suture, non-absorbable),

— if appropriate, that the suture is coloured,

— if appropriate, the structure (braided, monofilament,

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